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Megalomania's Controversial Chem Lab 







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(^ 3^9 



Welcome to the Controversial Chem Lab. Here at the Chem Lab you 
can find information on a large number of chemicals that have a 
certain stigma attached to them. Chemicals such as explosives, drugs, 
and pesticides are vitally important for the survival of our civilization. 
Unfortunately, the scientific elite jealously hoards the knowledge on 
using and preparing these chemicals. Adding to the confusion is the 
scientific ignorant who fear chemistry and think these chemicals are 
dangerous. As my chemistry professor used to say about what they 
think, "chemistry equals bad." 

The Controversial Chem Lab was created to be a free reference on 
how to synthesize chemicals. It is also a virtual laboratory skills 
manual, complete with descriptions on how to conduct laboratories, 
and a visual database on many different kinds of laboratory apparatus. 
While the Chem Lab is written for the non-chemist audience, it does 
require a basic understanding of laboratory skills. Of course, all of the 
information needed to acquire a basic understanding of lab skills is 
included within the site. 

The Chem Lab even goes the extra mile in providing information on 
how to synthesize many of the chemicals used in making explosives, 
etc. It also provides information on where to acquire certain chemicals 
and apparatus. While all of this information is perfectly legal, it may be 
against the law in certain areas to prepare some of these chemicals 
without the proper license. 



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■2004 17:21:55 






Megalomania's Controversial Chem Lab 



To find your way through the site, just use the navigation bar at the 
left of the page. Each section is organized to provide more details as to 
what it contains, and has more navigational choices. 

The Controversial Chem Lab is the work of only one man, so please 
do not be surprised if some information is incomplete. This is a work in 
progress with no end in sight. If you find any inaccurate or incomplete 
information, please email me as soon as you can with the correct data. 

I may be conacted via the Roque Science contact forms . Every attempt 
has been made by me to insure the accuracy of all information, but 
there are always mischievous computers that like to change things for 
their twisted pleasure. If you feel that you have some valuable 
information to add to this website, please drop me a line. Watch out, 
you might learn something here. 

Megalomania's Controversial Chem Lab ©1997-2004 /homepage/ revised December 24, 2003 
Last Site Revision March 11, 2004 



http://www.roguesci.org/megalomania/index.html (2 of 2)12- 



■2004 17:21:55 



Megalomania's Explosives Section 




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(^ 3^9 



This section contains detailed information on how to synthesize 89 
different explosive compounds in the lab. With the exception of two or 
three mixtures, every one of these explosives is a unique molecular 
substance. These labs range from common explosives used by the 
military and industry, to rare rocket and shell propellants, to recently 
discovered experimental explosives. Although quite large compared to 
other Internet resources, this list represents only a tiny fraction of all 
explosive compounds. 

Each of the labs contained herein should only be performed by a 
person thoroughly familiar with proper laboratory technique. It is also 
illegal to prepare any explosive without a license. Although any 
chemistry lab can be dangerous, the nature of these chemicals is such 
that the dangers are exacerbated because they are explosives! Strict 
adherence to all instructions, and safety procedures is strongly 
recommended. 

Just click on the links in the following alphabetized index to get to 
the lab of your choice. Each explosive lab is arranged with a table 
highlighting certain physical characteristics, a little bit of background 
on the explosive, a table listing all of the equipment and chemicals 
that are needed in its preparation, and finally the method of synthesis 
itself. The initial mention of any chemical or apparatus is linked to its 
relevant section elsewhere in the site. 

Acetone Peroxide 
Allyl Hydroperoxide 
Ammonium Nitrate (§> 



Ammonium Picrate 



Astrolite 



Benzalaminoquanidine Nitrate 

a-Benzenediazobenzyl Hydroperoxide 

DADNBU 

DADNPE 

DDNP 



Dinitrobenzene 



Dinitrochlorobenzene @ 
Dinitropolystyrene 



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Megalomania's Explosives Section 



DNPA (•> 

EGDN 
FOX- 7 

Guanidine Carbonate 
Guanidine Nitrate @ 

1,1,1,3.5.5,5-Heptanitropentane 

Hexamethylenetetramine Dinitrate 

Hexanitrocarbanilide 

Hexanitrodiphenylamine 

HMTD 

HMX 

HNIW 

HNO 

IPN 

Lead Azide 

Lead Nitratophosphite 
Lead Picrate 
Lead Styphnate 

Lead 2,4,6-Trinitro-3-Oxybenzoate 

Maltose Octanitrate 

Mannitol Hexanitrate 

MEDINA 

MEDNA 

MeEDNA 

Mercurous Nitratophosphite 

Mercury Fulminate 

2-Methyl-2-Nitro-l-Propanolnitrate 

Metriol Trinitrate 

MMAN 

NIBGkDN 

NIBGTN 

Nitrated Petroleum 

m- Nitrobenzenediazonium Perchlorate 

2-Nitro-2-(3,5-dinitrophenvl)-propanediol-1.3 Dinitrate 

Nitrogen Sulfide 

Nitrogen Trichloride 

Nitrogen Triiodide 

Nitroglycerin 

Nitroguanidine (•> 

2- Nitro- 2- (m-Nitrophenyl)- Propanediol- 1,3 Dinitrate 
Nitrosoguanidine 



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Megalomania's Explosives Section 



Nitrostarch 

Nitrosyl Perchlorate 

NONA 

NPN 

NTN 

Perchlorates 
N-Perchlorvlpiperidine 
PETN 
Petrin @ 

Petrin Acrylate 
PGDN 

1- Phenyl- 2- Nitro-l-Propene 

Picric Acid (§> 

m-Picrylpicryl Chloride 

The Polymer 

Potassium Picrate 

Propylpicrate 

PVN 

RDX 

Silver Fulminate 

TACC 

TeNN 

Tetracene 

Tetranitromethane (§> 

Tetryl 
TNO (§> 

TNPEN 

TNPht 

Trinitroanisol 

Trinitrobenzene 

Trinitro-m-Cresol 

Trinitromethane 

2,4,6-Trinitro-m-Phenylenediamine 
l.l.l-Trinitro-2-Propyl Acrylate 
Trinitrostilbene 
Trinitrotoluene 

Tris[l,2-Bis (Difluoramino)-Ethyll Isocvanurate 



The icon indicates an explosive that can be used to make other explosives. 



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Megalomania's Explosives Section 



Megalomania's Controversial Chem Lab ©1997-2004 /explosives/ revised January 31, 2004 



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Chemical Weapons and Poisons 



#1 was in the middle of converting this to XHTML 9- 1 8-02 




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The chemical weapons section is supposed to have varied methods of laboratory 
synthesis for some of the deadliest chemicals known to man. Not only do these include 
your standard war gasses, but also poisons. I say supposed to have because I don't 
actually have any information ready for posting on the web yet. While I have acquired 
much valuable data, it still needs to be edited and converted to a web format. The 
following list of substances represents the information that I have synthesis data for. 

Acrolein 

Benzyl Bromide 

Benzyl Chloride 

Benzyl Iodide 

Bromoacetone 

Bromoacetophenone 

Bromobenzyl Cyanide 

Bromopicrin 

Carbon Monoxide 

Carbonyl Bromide 

Chloroacetone 

Chloroacetophenone 

Chloroformoxime 

Chloromethyl Chloroformate 

Chloropicrin 

Chlorosulfonic Acid 

* checked to here* Cyanogen Bromide 

Cyanogen Chloride 

Cyanogen Fluoride 

Cyanogen Iodide 

Cyclosarin 

Cyclosoman 

Dibromoacetylene 

Dibromomethyl Ether 

Dibromoethyl Sulfide 

Dichloroethyl Sulfide 

Dichloroformoxime 

Dichloromethyl Chloroformate 

Dichloromethyl Ether 

Diiodoacetylene 

Diiodoethyl Sulfide 

Dimethyl Sulfate 

Diphenyl Chloroarsine 

Diphenyl Cyanoarsine 

Ethyl Bromoacetate 

Ethyl Chloroacetate 

Ethyl Dihloroarsine 



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Chemical Weapons and Poisons 



Ethyl lodoacetate 
Hexachloromethyl Carbonate 
Hydrocyanic Acid 
Lewisite 

* Methyl Chloroformate 
Methyl Chlorosulfonate 
Methyl Dihloroarsine 
Methyl Fluorosulfonate 
Methyl Formate 
Methyl Sulfuric Acid 
Oxalyl Chloride 
Perchloromethyl Mercaptan 
Phenarsazine Chloride 
Phenyl Carbylamine Chloride 
Phenyl Dichloroarsine 
Phosgene 
Sarin 
Soman 

Sulfuryl Chloride 
Tabun 

Tetrachlorodinitroethane 

Thiophosqene 

Thiosarin 

Thiosoman 

Trichloromethyl Chloroformate 
Trichloro Nitroso Methane 
VX 

Xylyl Bromide 

Megalomania's Controversial Chem Lab ©1997-2004 /chemical weapons/ revised January 31, 2004 



http://www.roguesci.org/megalomania/chemwep.html (2 of 2)12-8-2004 17:22:01 



Megalomania's Pharmaceutical Section 




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Weapons 


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» 


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The pharmaceutical section is supposed to have varied methods of 
laboratory synthesis for recreational drugs, and prescription medication. I may 
even throw in info for fermenting beer and liquors. I say supposed to have 
because I don't actually have any information ready for posting on the web 
yet. While I have acquired some valuable data, I have other projects to get 
done first. Try a few of the links below to get started. 

Check Out These Links! 

Rhodium - an informative element 
lohan's Guide to Aphrodisiacs 
The Hypereal Drug Archive 
The Lycaeum 
The Vaults of Erowid 



Megalomania's Controversial Chem Lab ©1997-2004 /pharmaceuticals/ revised January 31, 2004 



http://www.roguesci.org/megalomania/pharm.htmll2-8-2004 17:22:02 




Megalomania's Pesticides Section 




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Weapons 


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» Disclaimer 


» Search this site 







This is a section for pesticides, herbicides, rodenticides, 
algaecides, indeed all of your favorite "cides" will be listed here. Many 
excellent pesticides have been banned over the years for dangers to 
the environment, or people, but were very effective. Certain modern 
"cides" are also rather expensive. This will not be a comprehensive of 
such chemicals, but it will contain a few choice ones. 



Megalomania's Controversial Chem Lab ©1997-2004 /pesticides/ revised January 31, 2004 



http://www.roguesci.org/megalomania/pest.htmll2-8-2004 17:22:03 




Megalomania's Precursors Section 




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Weapons 


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» Precursors 


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» Lab Equipment 


» Safety 


» Roque Science 


» Links 


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» Contact Me 


» Disclaimer 


» Search this site 







A precursor is a chemical substance that is used to synthesize an 
explosive, poison, drug, etc. This section of the Controversial Chem 
Lab is here to provide useful information on all of the chemicals used 
in the various procedures throughout the website. Here you can find 
information on the important physical properties of many compounds. 
There is also a material safety data sheet (MSDS) for just about every 
chemical, as well as storage suggestions. Most important of all, this 
section contains complete synthesis information for most of the 
chemicals here. 

One of the largest problems facing the hobbyist today is the lack 
of vendors willing to sell chemicals to those without a business or 
school purchase order. There are also very few companies willing to 
sell small quantities of chemicals. When a company does sell in small 
quantities, the chemical is usually of high quality, and thus adds a 
considerable sum to the price. Then there are the excessive 
government regulations on hazardous substances, which of course 
mean special shipping procedures, and ultimately even more expense. 

The fact is there is simply not enough market demand from 
individuals for chemicals nowadays. Remember that it is perfectly 
legal to own just about any precursor, it is how the chemicals are 
used that you can run afoul of the law. Within this section is sufficient 
information for you to make your own chemicals, or where to get the 
chemicals that you cannot make. All of this can be done without the 
prohibitive cost of ordering through a chemical supplier. To the best 
of my knowledge there is no other project like this one on the 
Internet. Please understand that this is a very daunting task, there is 
a reason no one else has ever done what I have here, it is a lot of 
work. Some chemicals will be difficult to make, perhaps impossible, 
but ordering one or two such chemicals from a supplier is better than 
dozens. 



This is the motto of the precursor section: 

The land beneath our feet, the air in our lungs, the trees on the 

horizon. 

All are sources of chemicals. 

No legislation can ban them, no government can control them, no 

soldier can take them. 

If industry can do it, so can I. 



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Megalomania's Precursors Section 



Chemicals and their Synonyms 



This index includes a link for every chemical used throughout the website. The links will take you to a 
page that has important information about the chemical as well as a detailed lab synthesis. All names in 
bold are the primary names used in the site, all other names are synonyms. 

aibicidieifigihiiijikiliminioipiqirisitiuiviwixiyiz 

A 



absolute alcohol 
ac 5230 
acardite 
acenterine 
acesal 

acetaldehyde 

acetamide 

Acetaminophen Aspirin 
acetate 

acetate salicylic acid 
acetic acid 
acetic acid amide 
acetic acid anhydride 
acetic acid chloride 
acetic acid ethyl ester 
acetic acid glacial 
acetic acid, lead(2+) salt 
acetic aldehyde 
acetic anhydride 
acetic chloride 
acetic ester 
acetic ether 
acetic oxide 
aceticyl 
acetidin 
acetilsalicilico 
acetilum acidulatum 
acetimidic acid 
acetisal 
acetone 



acrylic acid chloride 

acrylic acid methyl ester 

acryloyl chloride 

acrylyl chloride 

activated carbon 

activated carbon, decolorizing 

activated charcoal 

acylpyrin 

Aerothene MM 

aethylis 

aethylis chloridum 

aglime 

Akwa Tears 

Albone 

A1C13 

alcohol 

alcohol dehydrated 

alcohol of sulfur 

alcojel 

alcosolve 

alcosolve 2 

aldehyde 

algrain 

Alka-Seltzer 

alluminio(cloruro di) 

allyl mesylate 

allyl methanesulfonate 

almond artificial essential oil 

4-O-alpha-D-glucopyranosyl-D- 

glucose 



ammonia water 
ammonioformaldehyde 
ammonium, aqueous 

ammonium carbonate 

ammoniumchlorid 

ammonium chloride 
ammonium ferrous sulfate 
ammonium hydroxide 

ammonium iron sulfate 

ammonium muriate 

ammonium sesquicarbonate 

amylum 

AN AC 110 

Anacin 

anesthetic ether 
anhydrol 

anhydrous alcohol 
anhydrous hydrazine 
anilin 
anilina 

aniline 

aniline hydrochloride 

aniline oil 
aniline reagent 
animal charcoal 
(6)annulene 
Anodynon 
antisal la 
anyvim 
aqua ammonia 
Aquacare/HP 



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Megalomania's Precursors Section 



aceto hmt 


4-(alpha-D-glucosido)-D-glucose 


Aquadrate 


acetonyl 


Altacide 


aqua fords 


acetophen 


aluminium 


aqueous ammonia 


acetosal 


aluminiumchlorid 


aragonite 


acetosalic acid 


aluminium, (chlorure d') 


artificial almond oil 


acetosalin 


aluminium trichloride 


artificial bitter almond oil 


2-acetoxybenzoic acid 


aluminum 


artificial essential oil of 


acetoxyethane 


aluminum chloride 


almond 


acetylaldehyde 


aluminum chloride (1:3) 


arwood copper 


acetyl anhydride 


amarthol fast orange r base 


arylamine 


acetyl chloride 


Amchlor 


A.S.A 


acetyl ether 


ameisensaure 


a.s.a. empirin 


acetylin 


aminic acid 


asagran 


acetyl oxide 


aminobenzene 


asatard 


2-(acetyloxy)-benzoic acid 


2-amino-4,6-dinitrophenol 


Ascoden-30 


acetylsal 


6-amino-2,4-dinitrophenol 


Ascriptin 


acetylsalicylic acid 


Aminoform 


ASH 


acetyl salycylic acid 


aminoguanidine bicarbonate 


aspalon 


Acid Mist 


aminoguanidinium hydrogen 


aspergum 


acidogen nitrate 


carbonate 


aspirdrops 


acidum acetylsalicylicum 


aminomethane 


aspirin 


Aci-Jel 


m-aminonitrobenzene 


Aspro 


aciletten 


1 -amino- 3 -nitrobenzene 


asteric 


acimetten 


aminophen 


atomite 


acisal 


2-aminopropane 


Augus Hot Rod 


acroleic acid 


Ammoform 


avantin 


acrylate 


ammoneric 


azide 


acryl chloride 


ammonia 


azium 


acrylic acid 


ammonia, monohydrate 


azobase mna 
azotic acid 



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Megalomania's Precursors Section 



ba 0108E 
baker's p and s 
baking soda 

barium chloride 

barium dichloride 
Basodexan 
benaspir 
bensulfoid 

benzal chloride 
benzaldehyde 
benzaldehyde 
phenylhydrazone 

benzalphenylhydrazine 

benzamine 

benzene 

benzene, amino- 

benzenecarbonal 

benzene carboxaldehyde 



Calcichew 

Calcidia 

calcined brucite 

calcined magnesia 

calcined soda 

Calcit 

calcite 

calcium carbonate 
calcium chloride 
calcium dichloride 
calcium dihydroxide 
calcium hydrate 
calcium hydroxide 
calcium hypophosphite 
calcium sulfate 



benzene chloride 

benzene methylal 

benzenol 

benzidam 

Benzin 

benzin 

benzine 

Benzinoform 

benzoic aldehyde 

benzol 

benzolene 

Benzoline 

benzoyl hydride 

benzyl dichloride 

benzylene chloride 

benzylidene chloride 

benzylidene dichloride 

benzylidenephenylhydrazine 

BFV 

bialpirinia 
bicarbonate of soda 

c 



carbonyl diamide 

carbonyldiamine 

carboraffin 

carborafine 

carboxide 

o-carboxyphenyl acetate 

caustic lye 

caustic potash 

caustic soda 

CPA 102 

CPA 122 

Celite 

chalcanthite 

chalk 



bicarburet of hydrogen 

bichromate of soda 

2,2-bis(hydroxymethyl)~ 1 ,3- 

propanediol 

blue oil 

blue powder 

bluestone 

blue vitrol 

Bonide Sulfur Plant 

Fungicide 

booze 

BOU 

brimstone 

British gum 

Brocide 

bromine 

bromobenzene 

Bufferin 

Bulbold 



C.I. oxidation base 1 
citretten 

citric acid 

Citrical 

Citro 

Clifton Sulfur 
cloretilo 
coal naphtha 
col-evac 
colfarit 
Colloidal-S 
colloidal sulfur 
Collokit 



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Megalomania's Precursors Section 



calcosan 


charcoal 


cologne spirits 


camphor tar 


charcoal, activated 


colonial spirit 


canary dextrin 


Chelen 


Colsul 


Canadol 


chevron acetone 


Columbian spirits 


caprin 


Chile saltpeter 


combi-schutz 


carbamaldehyde 


chlorate of soda 


common salt 


carbamide 


Chlorax 


contrheuma retard 


carbamimidic acid 


chlorene 


copper 


carbanilide 


chlorethvl 


copper sulfate 


carbinamine 


chloric acid, sodium salt 


cordycepic acid 


carbinol 


chlorid amonny 


Coricidin 


carbolic acid 


chlorid kvselinv akrylove 


Coricidin D 


carbon 


chloridum 


corn dextrin 


carbon, activated 


chlorinated water 


Coro sal D and S 


carbon, activated or decolorizing chlorine 


Cosan 


carbon, amorphous 


chloroacetic acid 


COSAN 80 


carbon black 


alpha-chloroacetic acid 


cr 


carbon decolorizing 


chlorobenzal 


cresol 


carbon dioxide 


chlorobenzene 


m-cresol 


carbona 


chlorobenzene mono 


cresylic acid 


carbon bisulfide 


chlorobenzol 


cresylol 


carbon bisulfuret 


chloroethane 


Cristal 


carbon chloride 


chloroethanoic acid 


crystal ammonia 


carbon disulfide 


chloroform 


Crystex 


carbone 


chlorohydric acid 


cubic niter 


carbonic acid, ammonium salt 


2-chloro -1,3, 5 -trinitrobenzene 


cupric sulfate 


carbonic acid calcium salt (1:1) 


Chlorpheninaurine 


curithane 103 


carbonic acid, diammonium salt 


chlorure d'aluminium 


CuTEA 


carbonic acid disodium salt 


chloryl 


cutrine-plus 


carbonic acid monosodium salt 


Chlorvl Anesthetic 


cyanoguanidine 


carbonic acid sodium salt (1:1) 


chromar 


1-cyanoguanidine 


carbonic acid, with 


C.I. 37030 


2-cyanoguanidine 


hydrazinecarboximidamide (1:1) 


C.I. 76000 


cyanol 


carbonio 


C.I. 77400 


cyclohexatriene 


carbon oil 


C.I. 77577 


Cystamin 


carbon sulfide 


C.I. azoic diazo component 7 


Cystogen 


carbon tet 


Cimcool wafers 





carbon tetrachloride 



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Megalomania's Precursors Section 



daito orange base r 

Darammon 

Darvon compound 

PCD 

PCM 

Pefol 

dehydrated alcohol 

denatured alcohol 

dendritis 

Pervan 

devol orange r 

dextrin 

dextrin hydrate, white 

diamide 

diamine 

diammonium carbonate 
diatomaceous earth 

2.3- diazido-l,4-butanediol 

3.3- diazido-2,4-pentanediol 

diazo fast orange r 
dibasic lead acetate 
dichlorine 

1 .2- dichloroethane 
sym-dichloroethane 
dichloromethane 

( dichloromethyljbenzene 
dichloro methyl-benzene 
dichlorophenylmethane 
a,a-dichlorotoluene 

1.3- dichloro-2, 4,6- 
trinitrobenzene 
dicyandiamide 
dicyanodiamide 
diethylene dioxide 

1 .4- diethylene dioxide 
diethylene ether 



D 



diethyl ether 

diethyl oxide 

N,N'-difenylmocovina 

dihydrogen dioxide 

dihydrogen monoxide 

1 ,2-dihydroxy ethane 

1 ,2-dihydroxy propane 

( dimethy laminojbenzene 

dimethylaniline 

N,N -dimethylaniline 

N,N-dimethylbenzenamine 

dimethylbenzene 

dimethylcarbinol 

N,N -dimethylformamide 

dimethyl formaldehyde 

dimethylketal 

dimethyl ketone 

dimethylphenylamine 

N,N-dimethylphenylamine 

dimethylphylamine 

dinitroaminophenol 

2.4- dinitro-6-aminophenol 
4,6-dinitro-2-aminophenol 
m-dinitrobenzene 
dinitrogen monoxide 
dinitrogen oxide 
dinitrogen tetrafluoride 

2.4- dinitrophenetole 
b-(2,4-dinitrophenoxy) ethanol 
dinitrophenylglycolether nitrate 
diokan 

Piosmol 

Piox 



1 .4- dioxacyclohexane 
dioxane 

1.4- dioxane 
p-dioxane 
dioxyethylene ether 
diphenylcarbamide 
N,N’-diphenyl-ethanediamide 
diphenylhydrazone 
diphenylurea 

1,3-diphenylurea 

1,3 -diphenylurea 
3 -diphenylurea 
N,N’-diphenylurea 
s-diphenylurea 
s ym- diphenylurea 
diphosphorus pentoxide 
dipping acid 
dipropyl 

disodium carbonate 

disulfur dichloride 

dithiocarbonic anhydride 

PMA 

PMF 

PMFA 

Powtherm 4000 
Powtherm SR 1 
Pri-Pie 

dried cupric sulfate 

Prop-Leaf 

Prysol 

dublofix 

duramax 

Putch liquid 

Pylene 



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Megalomania's Precursors Section 



diethylene oxide 
1 ,4-diethy leneoxide 



ECM 

Ecotrin 

EDC 

EG 

Elosal 

Elvanol 

empirin 

endydol 

entericin 

enterosarine 

entrophen 

erinitrit 

essence of mirbane 
essence of myrbane 
ethanal 
ethanamide 
1 ,2-ethanediol 



factitious air 
Fall 

fannoform 
fast orange base r 
fast orange m base 
fast orange mm base 
fast orange r base 
fermentation alcohol 
ferrous ammonium sulfate 
flowers of sulfur 
flour sulfur 



E 

ethane- 1,2 -diol 
ethanoic acid 
ethanoic anhydrate 
ethanoic anhydride 
ethanol 

ethanol 200 proof 
ethanoyl chloride 
ethenol homopolymer 
ether 

ether chloratus 
ether hydrochloric 
ether muriatic 
ethoxyethane 
ethyl acetate 
ethyl acetic ester 
ethyl alcohol 
ethyl aldehyde 
ethylaldehyde 

F 

flukoids 

Formagene 

formaldehyde 

formaldehyde solution 
Formalin 
Formalin 40 
formalith 

formamide 
formamine 
formic acid 

G 



ethyl chloride 

ethylene alcohol 

ethylenecarboxylic acid 

ethylene chloride 

ethylene dichloride 

ethylene dihydrate 

ethylene glycol 

ethylene glycol ethylene ether 

ethyl ether 

ethyl hydrate 

ethyl hydroxide 

ethylic acid 

ethyl oxide 

Excedrin 

extra fine 200 salt 

extra fine 325 salt 

extren 



formic aldehyde 
formimidic acid 
Formin 
Formol 
formylic acid 
formyl trichloride 
fossil flour 
Freon 30 
Fridex 

fuming nitric acid 
FYDE 



http://www.roguesci.org/megalomania/synthesis.html (7 of 17)12-8-2004 17:22:07 



Megalomania's Precursors Section 



gas 


Glauber's salt 


gasahol 


Glyceol 


gasolene 


glycerin 


gasoline 


glycerine 


Gelprin 


glycerin mist 


Gelvatol 


glyceritol 


gettysolve-b 


glycerol 


glacial acetic acid 


D- glycerol 



L-glycerol 

glycol 

glycol alcohol 

glycoldinitrophenylether 

nitrate 

glycol ethylene ether 
glycyl alcohol 
Golden Dew 
GOX 

grain alcohol 



halite 


hexyl hydride 


hydrochloride 

hydrocyanite 

hydrogen 

hydrogencarboxylic acid 
hydrogen chloride 


hard paraffin 


h.g. blending 


hydrogen dioxide 


hartosol 


high-strength hydrogen peroxide 


hydrogen nitrate 


hartshorn 


hiltonil fast orange r base 


hydrogen oxide 


Harvest-Aid 


Hioxy 


hydrogen peroxide 


HBIW 


Hiprex 


hydrogen sulfate 


HCHO 


HMT 


hydroperoxide 


helicon 


HMTA 


hydroxybenzene 


Hercules P 6 


H202 


2-hydroxy-3,5-dinitroaniline 


Hex 


HOCH 


hydroxymethyl)-2- 


HEXA 


hooch 


nitropropanediol 


Hexaform 


Huile D'aniline 


hydroxymethyl) -2- 


hexahydropyridine 


Hyanit 


nitropropane- 1 ,3-diol 


hexamethylenamine 


hydrargyrum 


2-hydroxymethyl-2- 


hexamethyleneamine 


hydrated lime 


nitropropanediol 


hexamethylenetetraamine 


hydrazine 


2-(hydroxymethyl)-2-nitro- 


hexamethylene tetramine 


hydrazine base 


1,3 -propanediol 


hexamethylene triamine 


hydrazine, hydrazine sulfate 


2-hydroxypropane 


hexamine 


hydrazine, tetrafluoro- 


hydroxy- 1,2,3- 


hexane 


hydrazoic acid, sodium salt 


propanetricarboxylic acid 


n-hexane 


hydrocerol a 


2-hydroxy- 1,2,3- 


Hexasul 


hydrochloric acid 


propanetricarboxylic acid 



http://www.roguesci.org/megalomania/synthesis.html (8 of 17)12-8-2004 17:22:07 



Megalomania's Precursors Section 



hexilmethylenamine 



IFP 

imsol a 

incorporation factor 

infusorial earth 

Inhibine 



jay sol 
jay sol s 



karbanilid 
karsan 
Kelene 
Keratinamin 
ketone propane 



hydrochloric ether 



I 

intergravin-orales 

iodine 

IPA 

i-propanol 

iron 

iron ammonium sulfate 
Irtran-5 

J 



Jodid 



K 

beta-ketopropane 

kieselguhr 

kohlendisulfid 

Kolofog 

Kolospray 

L 



hydroxytricarballylic acid 
2-hydroxytricarballylic acid 
beta-hydroxytricarballylic 
acid 

hyponitrous acid anhydride 



isohol 

isopropanol 

isopropyl alcohol 
isopropylamine 

isourea 



jusonin 



komeen 

koolstofdisulfide 
krystallin 
Kumulus S 
kyanol 



http://www.roguesci.org/megalomania/synthesis.html (9 of 17)12-8-2004 17:22:07 



Megalomania's Precursors Section 



laughing gas 

lead acetate 

lead diacetate 
lead dibasic acetate 
lead dinitrate 
lead monoxide 
lead nitrate 
lead (II) nitrate 
lead ocher 
lead oxide 
lead (II) oxide 



macrogol 400 bpc 

Magcal 

Maglite 

magnesia 

magnesia usta 

magnesium monoxide 

magnesium oxide 

magnesium oxide, heavy 

magnesium oxide, light 

magnesium styphnate 

Magnetic 6 

Magnetic 70 

Maizena 

maltobiose 

Maltos 

maltose 

alpha-maltose 

D-(+)-maltose 

malt sugar 

Mandelamine 

Manicol 

manna sugar 



lead oxide (mono) 

lead oxide yellow 

lead protoxide 

lead(II) salt acetic acid 

Lensan A 

light gasoline 

ligroin 

ligroine 

lime, hydrated 

limestone 

lime water 

M 



liqueur 
liquid silver 
Liquifilm 
litharge 

litharge yellow L-28 

LOX 

lutosol 

lutrol-9 

lye 

lysoform 



mercury pernitrate 

Methacide 

methamin 

Methan 21 

methanal 

methanamide 

methanamine 

methanecarboxamide 

methanecarboxylic acid 

methane dichloride 

methanesulfonic acid, allyl ester 

methanesulfonic acid, 2-propenyl 

ester 

methane tetrachloride 



methane trichloride 
methanoic acid 
methanol 

methenamine 
metheneamine 
methenyl trichloride 
methoxycarbonylethylene 

3-methoxy-2,2 1 ,4,4 ' ,6,6 ' - 
hexanitrobiphenyl 
methyl acrylate 
methyl alcohol 



methyl propenoate 

methyl 2-propenoate 

methyl trichloride 

metriol 

meylon 

Microflotox 

mighty 150 

mighty rdl 

mineral naphtha 

mirabilite 

Mirasept 

mirbane oil 

Mohr's salt 

molasses alcohol 

molecular chlorine 

Mondamin 

monobromobenzene 

monochloroacetic acid 

monochlorobenzene 

monochlorobenzol 

monochloroethane 

monochloroethanoic acid 

monoethylene glycol 



http://www.roguesci.org/megalomania/synthesis.html (10 of 1 7 ) 1 2-8-2004 17:22:07 



Megalomania's Precursors Section 



Mannidex 


methyl aldehyde 


monohydroxy benzene 


mannite 


methylamine 


monohydroxymethane 


mannitol 


methylbenzene 


monoisopropylamine 


D-mannitol 


methyl-benzene 


monomethylamine 


marble 


methylbenzol 


monomethyl benzene 


Marcero 


methylcarbinol 


mononitrogen monoxide 


Martos-10 


methylene bichloride 


monopentaerythritol 


massicot 


methylene chloride 


monophenol 


Massicotite 


methylene dichloride 


monosodium carbonate 


MCA 


methylene glycol 


monosodium hydrogen 


MCB 


methylene oxide 


carbonate 


Measurin 


methyl ester acrylic acid 


moon shine 


M.E.G. 


methyl glycol 


Morbicid 


mercurialin 


methyl hydroxide 


mothballs 


mercuric nitrate 


methyl ketone 


moth flakes 


mercuric oxide 


2-methyl-2-nitropropane- 1 ,3-diol 


motor benzol 


mercury 


2-methyl-2-nitro-l,3- 


motor fuel 


mercury nitrate 


propanediol 


motor spirits 


mercury (II) nitrate 


2-methyl-2-nitropropanol 


Mowiol 


mercury oxide 


2- methyl-2-nitro-l-propanol 

methylol 

3- methylphenol 

N 


muriatic acid 
muriatic ether 



NaCl 

naphthalene 

naphthanin 
naphtha petroleum 
naphtha, VM&P 
naphthene 

naphtoelan orange r base 

Narcotile 

narkotil 

nitrate of soda 

natrium 

natron 



niter 

nitric acid 

nitric acid, lead(2+)salt 
nitric acid, mercury salt 
nitric acid, potassium salt 
nitric acid red fuming 
nitric acid, sodium salt 
nitric oxide 
nitroallyl acetate 
m-nitroaminobenzene 
3-nitroanaline 
3-nitroanihne 
m-nitroaniline 
3-nitrobenzenamine 



nitroisobutylglycerine 
nitroisobutylglycerol 
nitromethane 
2-nitro-2-methyl- 1,3- 
propanediol 

2-nitro-2-methylpropanol 
2-nitro-2-methyl- 1 -propanol 

2-nitro-2-(m-nitrophenyl)- 

propanediol-1,3 

m-nitrophenylamine 

1- nitropropane 

2- nitropropane 

nitrosonium tetrafluorborate 
nitrosyl fluoborate 



http://www.roguesci.org/megalomania/synthesis.html (11 of 1 7 ) 1 2-8-2004 17:22:07 



Megalomania's Precursors Section 



natural gasoline 


nitrobenzene 


nitrosyl fluoride 


NCI-C03736 


nitrobenzol 


nitrosyl tetrafluoroborate 


NCI-C04591 


nitrocarbol 


nitrotris (hydroxymethyl) 


NCI-C61074 


2-nitro-2- (3 ' ,5 ' -dinitropheny 1) - 


methane 


Necatorina 


propanediol- 1,3 


nitrous acid sodium salt 


necatorine 


nitroetan 


nitrous oxide 


NEUT 


nitroethane 


nitryl hydroxide 


neutral lead acetate 


nitrogen 


NM 


nevite 


nitrogen dioxide 


NMPD 


N2F4 


nitrogen fluoride 


NO 


N-H 


nitrogen monoxide 


N02 


Nital 


nitrogen oxide 


Norgesic 


nitranilin 


nitrogen peroxide 


norkool 


m-ni tramline 


nitro-2-(hydroxymethyl)- 1 ,3- 


normal hexane 


nitration benzene 


propanediol 


normal lead acetate 


3 -nitrazabuty lamine 


2-nitro-2-(hy droxymethyl)- 1,3- 


NSC 143016 




propanediol 

o 


NSC 37088 
Nutraplus 


oil of bitter almond 


Optal 


oxomethylene 


oil of mirbane 


orange base irga 1 
Osmitrol 


oxybenzene 


oil of myrbane 


l,l'-oxybisethane 


oil of vitriol 


oxalic acid 


Oxydol 


oleum 


oxaldianilide 


oxygen 


Onychomal 


nvQtiilirlp 


oxymethylene 


Ophthalgan 


UAttlllllViV/ 

oxomethane 


Oxysept 



P 



http://www.roguesci.org/megalomania/synthesis.html (12 of 1 7 ) 1 2-8-2004 17:22:07 



Megalomania's Precursors Section 



PAC (salt) 


phenyl chloride 
phenyl hydrate 




paracetaldehyde 


phenyl hydride 


precipitated 


paraffin 


phenyl hydroxide 


precipitated silica 


paraffin wax 


phenylic acid 


premium 


Parafomi 


phenylic acid, phenyl hydroxide 


preparation af 


paraformaldehyde 


phenylic alcohol 


pronarcol 


Paral 


phenylmethanal 


2-propanamine 


paraldehyde 


phenylmethane 


propan-2-amine 


Pastaron 


phenyl methane 


1 -propanol 


PE 200 


N-phenyl-N'-phenylurea 


2-propanol 


pearl ash 


phosphoric anhydride 


propan-2-ol 


Pearlman's catalyst 


phosphorus 


n-propan-2-ol 


Pearsall 


phosphorous pentoxide 


propanone 


Pegasyl 


phosphorus chloride 


1,2-propanediol 


pentaertyhrito 


phosphorus oxychloride 


propanetriol 


pentaerythritol 


phosphorus trichloride 


1,2,3-propanetriol 


perchloric acid 


phosphoryl chloride 


2-propanone 


perchloromethane 


picramic acid 


propene acid 


perchloryl fluoride 

perfluorohydrazine 


picraminic acid 

picryl chloride 


2-propenoic acid 


propenoic acid 


Perhydrol 


pigment metal 2 


2-propenoic acid methyl ester 


Peroxan 


pigment yellow 46 


propenoic acid methyl ester 


peroxide 


piperidine 


2-propenoyl chloride 


Persistin 


plumbous oxide 


propenoyl chloride 


PETP 


polyhydric alcohols 


propol 


petrohol 


polyoxymethylene 


n-propyl alcohol 


petrol 


polystyrene 


propylene glycol 


petroleum ether 


polyvinal alcohol 


propylic alcohol 


petroleum naphtha 


Polyviol 


protium 


petroleum spirits 


potassa 


Purex 


phene 


potassium carbonate 


PVA 


phenic 


potassium dinitroethanol 


pyridine 


phenic acid 


potassium hydrate 


pyroacetic acid 


phenol 


potassium hydroxide 


pyroacetic ether 


phenol alcohol 


potassium hypophosphite 


pyrobenzol 


phenylamine 


potassium iodide 


pyrodextrin 


phenyl bromide 


potassium nitrate 


pyroxylic spirit 



http://www.roguesci.org/megalomania/synthesis.html (13 of 1 7 ) 1 2-8-2004 17:22:07 



Megalomania's Precursors Section 



quick silver 
R 10 (refrigerant) 

R 20 (refrigerant) 

R 30 

Raney copper 
Rathje 

Rcra waste number P022 
Rcra waste number U012 



salacetin 
sal ammonia 
sal ammoniac 
salammonite 
salcetogen 
saletin 

salicylic acid acetate 
saline 

saline solution 
salmiac 
Salpetersaure 
sal soda 
salt 

salt cake 

salt of Saturn 

salt of tartar 

saltpeter 

Salzburg vitrol 

Santar 

SBA0108E 

schwefelkohlenstoff 

sd alcohol 23-hydrogen 

sea salt 

sec-propanol 



potato alcohol 



Q,R 



Red Devil Lye 
red fuming nitric acid 
red mercury (II) oxide 
refined solvent naphtha 
refrigerant RIO 
refrigerant R20 
Refrigerant 30 
Resectisol 

s 



soda ash 
soda chlorate 
soda lye 
soda mint 
soda niter 
sodium 

sodium acetate 
sodium acid carbonate 
sodium acid sulfate 
sodium acid sulfite 
sodium azide 
sodium benzoate 
sodium bicarbonate 
sodium bichromate 
sodium bisulfate 
sodium bisulfite 
sodium carbonate 
sodium chlorate 
sodium chloride 
sodium dichromate 
sodium hydrate 
sodium hydrocarbonate 
sodium hydrogen carbonate 
sodium hydrogen sulfate 
sodium hydrogen sulfate 



resotropin 
Rfna 
rhodine 
Robaxisal 
rock salt 
Roman vitrol 
rubbing alcohol 



Spersul thiovit 
Spirit of Hartshorn 
spirits 

spirits of salts 

spirits of wine 

starch 

starch gum 

stat trak plus 

sterisol hand disinfectant 

sterling 

styrofoam 

sugar of lead 

Sul-Cide 

Sulfex 

Sulfidal 

sulfocarbonic anhydride 

sulfolane 
Sulforon 
sulfur 
sulfur acid 
sulfur atom 
sulfur chloride 
sulfur dichloride 
sulfur, flowers 
sulfuric 



http://www.roguesci.org/megalomania/synthesis.html (14 of 1 7 ) 1 2-8-2004 17:22:07 



Megalomania's Precursors Section 



sec-propyl alcohol 
sec-propylamine 
Security Nutronex 
Sefril 

Shed-A-Leaf 'L' 
shotgun 
silica gel 
siliceous earth 

silicic acid 
silver 

silver iodide 
silver nitrate 

skellysolve B 
slaked lime 
slaker rejects 
smite 
Sno Tears 
soda 



monohydrate 

sodium hydroxide 
sodium hypochlorite 
sodium nitrate 

sodium (I) nitrate 

sodium nitrite 

sodium pyrosulfate 

sodium sulfate 

sodium sulfite 

Sofril 

solaesthin 

solfuro di carbonio 

solmethine 

soludal 

Solvay soda 

solvent naphtha 

spectrar 

Sperlox-S 

Spersul 

T 



table salt 


tetrasol 


takineocol 


That F 


tar camphor 


thenardite 


TCLP extraction fluid 2 


thermonatrite 


tecsol 


Thiolux 


tescol 


Thion 


Tesuloid 


THION 80 


1 ,3,5,7-tetraazaadamantane 


THION 95 


1,3, 5 ,7-tetraazatricy clo 


thionyl chloride 


[3.3.1.l27]decane 


thiophan sulfone 


tetraazatricyclo[3.3. 1.1(3, 7)1 


Thiorit 


decane 


Thiovit 


tetrachlorocarbon 


THME 


tetrachloromethane 


Thyroblock 


tetrafinol 


Thyrojod 


tetrafluorhydrazine 


tin 


tetraform 


tol 



http://www.roguesci.org/megalomania/synthesis.html (15 of 1 7 ) 1 2-8-2004 17:22:07 



sulfuric acid 

sulfuric acid, ammonium iron 
(2+) salt 

sulfuric acid, monosodium 
salt 

sulfuric ether 

sulfur monochloride 

sulfurous oxychloride 

sulfur subchloride 

Sulkol 

Sulsol 

Supac 

super 

Super-Cel 

Super colloid 

Super Six 

superlysoform 

superoxol 

Synasol 



Triaminicin 

trichloroaluminum 

trichloroform 

trichloromethane 

tricresol 

trifluoroacetic anhydride 

triformol 

trihydroxypropane 

1,2,3-trihydroxypropane 

trimethylolnitromethane 

2,4,6-trimethyl-l,3,5-trioxane 

trinitro-m-anisidine 

trinitro-m-phenetidine 

trioxymethylene 

tris(hydroxymethyl) 

nitromethane 



Megalomania's Precursors Section 



tetrahydro- 1 ,4- dioxin 


toluene 


tris-nitro 


tetrahydro-p-dioxin 


toluol 


trivinyl isocyi 


tetrahydrothiophene 1,1 -dioxide 


tolu-sol 


Try cite 


tetrahydrothiophene 1 -dioxide 


m-tolylboronic acid 


t- stuff 


tetrakis (hydroxy me thy l)methane 


top flake 


Tumbleaf 


tetramethylolmethane 


torrefaction dextrin 

u 




U-3886 


ucar 17 


unleaded 


Ureophil 


UN 1131 


urea 


Urepearl 


UN 1547 


urea, 1,3 -diphenyl- 


UREX 


UN 1726 


urea nitrate 


Uritone 


UN 1955 


Ureaphil 


Uroqid 


UN 7581 


Urecare 


Urotropin 


univerm 


Urederm 


USAF ek-534 



Vanquish 

varnish makers' & painters' 

naphtha 

vaterite 

Veracur 

vermoestricid 



washing soda 
water 
weeviltox 
wegla dwusiarczek 
white crystal 



V 



Versneller NL 63/10 

Vinarol 

vinegar 

vinegar acid 

vinegar naphtha 



W 



white caustic 
white dextrin 
white tar 
whiting 



Vinol 

vinylformic acid 
vitriol brown oil 
V.M.&P. naphtha 



wood 

wood alcohol 
wood naphtha 
wood spirit 



X, Y, Z 



XAXA 

xylene 

xylol 



yellow dextrin 
yellow lead ocher 
yellow mercury (II) oxide 



yellow oxide of mercury 

zinc 

Zolvis 



aibicidieifigihiiijikiliminioipiqirisitiuiviwixiyiz 



http://www.roguesci.org/megalomania/synthesis.html (16 of 1 7 ) 1 2-8-2004 17:22:07 



Megalomania's Precursors Section 



Chemical Table Reference 





Chemical Name 


Chemical 

Formula 


List Number 


Molecular image 

X 

W-/K 
z 1 

unknown 


mp=melting bp=boiling d= 

point point 


m=molecular 

mass 


c $?.??=cost 




Safety Data: Material Saftey Data Sheet 


ChemAlcrl* 

. Siorgge Code 

GfiAY 


Synonyms: Alternative names of the compound 


Synthesis: This portion describes either how to synthesize the compound or where to obtain the 
compopund 



Synthesis Section Nav-Bar 

Page UPage 2 I Page 3 I Page 4 I Page 5 

Megalomania's Controversial Chem Lab ©1997-2004 /precursors/ revised March 11, 2004 



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Megalomania's Lab Skills Section 




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This page, when done, will contain an descriptions, as well as 
pictures, for every little chemistry technique and definition uson on 
the site. Consider this page a complete college lab text with all you 
will ever need to know. Whenever a technique is used, a setup called 
for, or a particular term mentioned there will be a link to the relative 
part of this section. It may help to read all of techniques here to gain 
a valuable insight into how to conduct an actual synthesis. There may 
also be some parts here that are not linked from elsewhere in the site. 

Try these links until I get done... 

Laboratory Encyclopedia 
Lab Skills 



These links are not very good, but hey, it's all I have considering this 
is a ton of work to do, and not a very high priority compared to other 
sections. There is not a lot of free information these days either. I will 
free it for you. 

Lab Skills 



adding 

collect 

cooling 

dissolving 

distillation 

drying 

evaporation 



acid 

alkaline 

base 

combustion 

concentrated 

crystals 

decomposition 

deflagration 

detonation 



extraction 

filtration 

fume removal 
pouring 
purification 
recrystallization 


refluxinq 

salt- ice bath 

stirring 

storing 

temperature 

washing 


Chemistry Terms 

dust 

grams 

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mixture 

moles 

pH 

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precipitate 

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reaction 

salt 

sensitivity 

sensitizer 

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Megalomania's Controversial Chem Lab ©1997-2004 /lab skills/ revised January 31, 2004 



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Megalomania's Lab Skills Section 



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Megalomania's Lab Equipment Section 




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This section is here to provide a visual description of every type of 
laboratory glassware, apparatus, and equipment that is required to 
perform a particular synthesis. Each piece of labware has a representitive 
picture as well as a description of what the object does, and where to get 
it. Since this section is still under construction it is not as informative as it 
could be. Pictures are provided, but not much in the way of descriptions. 

The following tables contain an alphabetical index of either glassware 
or apparatus. Whenever a piece of labware is mentioned in any lab, there 
is a direct link to the respective component. It may to helpful to 
familiarize yourself with all of the labware here before attempting any 
procedure. 

Glassware 



Adapters 

Beakers 

Bottles 

Bubblers 

Burets 

Condensers 

Crucibles 



Dishes 

Distilling Columns 
Drying Tubes 
Flasks 
Funnels 

Graduated Cylinder 



Mortar and Pestle 
Pipets 

Stirring Rods 
Test Tubes 
Tubing 
Watch Glass 



Apparatus 



Apron 

Aspirator 

Brushes 

Burners 

Clamps 

Desiccators 

Filter Paper 

Gloves 



Goggles 
Flotplate 
Magnetic Stirrer 
pFH Paper 
Pipet Bulbs 
Pipestem Triangle 
Ringstand 
Rings 



Stoppers 

Test Tube Clamp 

Test Tube Rack 

Thermometer 

Tongs 

Tubing 

Wash Bottle 



Try out the LabVista Web Search Engine! 

Search hundreds of used equipment dealers web pages to find virtually any type of labware. 

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Megalomania's Controversial Chem Lab ©1997-2004 /lab equipment/ revised January 31, 2004 



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Megalomania's Safety Section 




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The possession and handling of chemicals, especially explosives, 
can be extremely hazardous to an untrained or ignorant individual. 

The preparation of any explosive or chemical substance requires a 
good deal of planning and forethought to be successful. 

To begin with, you should have a dedicated area to set up your lab 
that has a sizable work area, easy access to chemicals and apparatus, 
seclusion from prying eyes, a minimum of flammable materials, and 
good ventilation. A garage or basement is better than a kitchen to 
keep contamination to a minimum, a shed or other separate building 
is ideal should a disaster occur. 

It is advisable to never work alone in the lab if you can. Also get 
some basic protective equipment such as gloves, aprons, goggles, 
and a respirator. It is best to have these things and wear them all the 
time because they can prevent a potentially harmful incident. Get 
some kind of fire extinguisher, big or little, its always best to get the 
kind that made for chemicals. A resourceful person may find that of 
all things fire extinguishers are found in public buildings just sitting on 
the walls waiting to be put to good use. Keep a garden hose at the 
ready as well as a bucket of water for emergency dilatation's or to 
douse yourself if (when) you catch fire, an extinguisher can be 
harmful to a person if sprayed onto them. 

Now chemical waste. I would suggest dumping chemical waste as 
far away from your property as possible. Dump it down a sewer, 
dump it on somebody's lawn, or just dump it near some industry and 
call the environmentalists to harass that company for spewing toxins, 
chances are that the environmentalists will already be there dumping 
toxins so they have something to complain about. Pay for professional 
disposal if you wish, but I believe environmental destruction is 
overrated. Dump it down the drain. 



Adapted from Safety In Academic Chemistry Laboratories, prepared by the American 
Chemical Society Committee on Chemical Safety, 1990. 

General: Never work in the laboratory alone. Perform no unauthorized experiments (A 
note if I may, its a good thing its your lab...) Do not use mouth suction to fill pipettes. 
Confine long hair and loose clothes while working in the laboratory. Wear shoes. Learn 
the location of and correct use of the nearest fire extinguisher. Learn the location of the 
safety shower and first aid kit and be prepared to give help to others (keep some means 



http://www.roguesci.org/megalomania/safety.html (1 of 2)12-8-2004 17:22:10 




Megalomania's Safety Section 



of running water ready and get some kind of first aid kit because minor accidents do 
happen, but they are usually more of a nusance than actually life threatning). 

Safety Glasses: Safety glasses should be worn at all times while in the laboratory, 
whether you actively engage in experimental work or not. Contact lenses should never 
be worn in the laboratory because they cannot be removed rapidly enough if reagents 
accidentally splash in the eye (I have seen it happen, chemical vapors tend to dissolve in 
the tears behind the lens and will not be flushed away, or a splash will trap chemicals 
behind and insure that it stays in direct contact with the cornea, ouch). 

Fire: Avoid unnecessary flames. Check the area near you for volatile solvents before 
lighting a burner. Check the area near you for flames if you are about to begin working 
with a volatile solvent. Be particularly careful of the volatile solvents diethyl ether, 
petroleum ether (ligroine), benzene, methanol, ethanol, and acetone. 

Chemicals: Handle every chemical with care. Avoid contact with the skin and clothing. 
Wipe up spills immediately, especially near the balances and regent shelf. Replace caps 
on bottles as soon as possible. Do not use an organic solvent to wash a chemical from 
the skin as this may actually increase the rate of absorption of the chemical through the 
skin. Avoid inhalation of organic vapors, particularly aromatic solvents and chlorinated 
solvents. Use care in smelling chemicals and do not taste them unless instructed to do 
so. Drinking, eating, or smoking in the laboratory is forbidden. 

Disposal of Chemicals: Dispose of chemicals as directed in each experiment. In 
general, small quantities of water-soluble substances can be flushed down the drain with 
a large quantity of water. Water-insoluble solids and liquids should be placed in the waste 
container provided. Chromium ion in the +6 oxidation state (orange) should be reduced 
to the +3 state (green) with a mild reducing agent such as bisulfate before disposal. 

Caution: It has been determined that several chemicals that are widely used in the 
organic laboratory (e.g., benzene and chloroform) cause cancer in test animals when 
administered in large doses (the good stuff always does this damnit). Where possible the 
use of these chemicals is avoided. I n the few cases where suspected carcinogens are 
used, the precautions noted should be followed carefully. A case in point is chromium in 
the +6 oxidation state. The dust of solid Cr+ 6 salts is carcinogenic. The hazards have 
been pointed out and safe handling procedures are given. 

Beware, this safety section is by no means completed yet. This is only a little of 
what I want to put here! 

Try this link for more safety information. 



Megalomania's Controversial Chem Lab ©1997-2004 /safety/ revised J anuary 31, 2004 



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Dear Forum members, 

As you are no doubt aware our presence on the web has 
unexpectedly come to an end. I want to dispel any rumors right 
now that this was the result of some government crackdown or 
that we are in any kind of legal trouble. It most certainly was not. Our service 
provider was pressured into closing our site by their service provider who was 
in turn threatened by a so-called group of crusading do gooders called 
iDefense. 

iDefense has made the absurd claim we are somehow involved with Arab 
terrorists. In fact their claims are pure lies. The actions of iDefense boarder on 
libelous, and if I had the money I would sue these misguided fools. They have 
tried to make an end run around the US Constitution and our guaranteed 
protections of free speech. Behind them I do suspect a government hand is at 
work, but since they have no legal basis to shut us down they use threats, 
intimidation, and outright criminal lies to trick our providers into shutting us 
down. 

While we may be shut out for a time, we are not silenced indefinitely. We 
will never rest and we will continue to exercise all of our freedoms in any way 
we see fit. We may be shut down again, but I will do everything in my power to 
make sure we return as soon as possible. 

There must now be a penalty applied to iDefense. There remains in my 
possession a considerable amount of knowledge concerning the synthesis of 
explosives and chemical weapons. I have held this knowledge in abeyance 
because I was unsure if the world is ready for it. I am the kind of person who 
does things solely for the reasons that others dislike it. Because iDefense 
thinks we have dangerous information I will no longer horde any of my chemical 
weapons information. I will distribute everything I have, and encourage others 
to do the same, for the very reason they don’t want me to. I will also make 
every effort to distribute our information in as many languages as possible, to 
as many websites as possible. 

There must be more of course. It has become necessary to establish 
additional websites in which to hold our knowledge. These will be created and 
kept secret until such a time as the main site goes down. I will also make 
available a complete archive of The Forum database which will be distributed to 
one and all. This archive will remain encrypted until we are forced to shut down. 
With the archive anyone will be able to recreate The Forum in its entirety, either 
starting your own website or running it on a PC. There will also be many more 
books made available via FTP sites, torrents, and other websites. I have also 
decided to expand the offerings of the Rogue Science website to include an 
additional forum. There must be additional outlets of discussion so we can draw 
an even greater audience from every nation of the world, even if those nations 
happen to be Arabic. 

A freedom you do not exercise will soon be taken away. They have fired the 
first shot in the war and in doing so they have aroused my ire. I was content in 
leaving things the way they were, but now I see complacency is the weakness 
our enemies want to exploit. Now that I know they are our to persecute us I will 
not rest until their every effort is thwarted. 



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Forum membership passes 10,000! 
July 15,2004 



The Explosives and Weapons Forum has been growing in leaps and bounds, 
and now we have finally reached our 10,000th member at the end of June. We 
are an overnight success 5 years in the making. Ahh, yes 5 years. July is the 
month I started the Forum back in 1999. July is also the anniversary of the 
Controversial Chem Lab, 2004 marks 7 years of my website. We are truly 
ancient by Internet standards. 

In other news the new unofficial FTP site has climbed to over 25 GB of content 
since it opened in April. Chemwarrior had a nervous breakdown because his 
platonic love was having intimate relations with everyone but him. The poor 
chap must have masturbation dementia and blue balls the size of grapefruit. 

In a stunning development the complete 2 CD set of The Encyclopedia of 
Explosives and Related Items volumes 1 to 10 is now available to one and all! 
Oh happy day. Retrosynthetic has been kind enough to convert it to a torrent 
for public download now that Rogue Science has its own torrent tracker. You 
may find the torrent file at the Filesoup torrent forums . You have to sign up to 
download the torrent, but it is an easy process. 



Forum outage. 

December^ 2003 

I knew it would happen sooner or later, and it finally did. The Forum database 
crapped out and the entire site shut down. Fortunately I was able to repair the 
database and restore the board right where it left off. Unfortunately it took me 
two days to do it. The cause? It may have had something to do with all that 
hacking I have been doing... 



Major changes to The Forum. 

December 1 . 7 ..2QQ2_ 

I have begun hacking the code in earnest this December since I have some 
free time. Now that I have had a chance to familiarize myself with the working 
of our board software I feel confident enough to make some much needed 
improvements. I hope our user experiences are improved from these changes. 
Most importantly newbies are prevented from starting new threads, hence we 
no longer have to ban them for this offence. Newbie threads are also 
moderated before going live to the world. There are many more changes to 
come in the weeks, and months, ahead. 




State of the site. 

■November 30, 2 Qfi3_ 

I know I have not updated the front page in some time, even though I have 
been changing it, I have not uploaded the changes. Most of the changes 
revolve around the new links engine, which as of this writing is almost ready to 
unveil to the world! I have changed the info on the unofficial FTP site to reflect 
its new ownership by chemwarrior, it's 30 GB and getting bigger all the time. I 
am thinking about opening a new section on The Forum just for FTP related 
stuff to encourage more people to run their own servers. Hopefully I can get 
someone to write a tutorial. 



The new site is under construction. 
SpjxyJ.OTtheJiist. . . 



The Rogue Science website has only begun to take shape. Most of the content 
you may see is merely place holding to get the look just right. I cannot really 
say how long it will be before some of the various sections are open for 
business, but they will be fleshed out over time. Keep a lookout for an index of 
explosives and other documents. We hope to offer some downloads and helpful 
instructions so that you can build your own explosive related website. Keep 
checking back for the latest updates! 



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Ever wanted to digitize your books to share them? How about 
protect your privacy online? Perhaps you have some information 
to share, but you don't know how to make your own website. The 
Rogue Science tutorials section is here to help. Below you will 
find an assortment of how-to guides designed to maximize the spread of 
information written by Forum members and staff. If you want to submit your 
own tutorial or how-to guide please use this handy form. 



Chem Lab 



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x Sometimes it helps to see what it is you are describing. Perhaps you 

have something interesting to show, or a design schematic that must be seen 
to be understood. Sometimes you don't want to go through the hassle of 
building your own website just to show a couple of snapshots. 

This tutorial takes you step by step through the process of creating your 
own free webspace just for hosting images. You can be online in a matter of 
minutes without learning web page creation, or using complex software. 



Library - by Ctrl C 



High Explosives 



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comprehensive link 
database now! The 
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Authored by: megalomania 



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You can use a digital camera to scan pages of a book, sometimes two 



Special Project 1 : Nitric 



pages at once, in a fraction of the time you could with a flatbed scanner. It is as 
simple as turn the page and take the picture. Devices that scan books this way 
are called planetary cameras, but the real things cost $20,000 and up! 

This tutorial shows you how you can use your digital camera to scan an 
entire book, and use software to process the images, so that you can make a 
quality digital copy of your books in less time than other methods. 



Issues and Opinions 



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Rogue Science - About the Staff 




Home 



The Rogue Science website is made possible by these individuals who have 
generously donated their time and effort to building the site into what it is today. 
Please take the opportunity to learn about who we are, what we do, and what 
our interests are. You will also be able to contact us here. 



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megalomania: The creator and webmaster of the Roque 
Science and Controversial Chem Lab websites as well as head 
administrator of The Explosives and Weapons Forum , 
megalomania is El Presidentae around here. 



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ilomania's PGP ki 



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Megalomania's Link Section 




Navigation 


» Home 


» Explosives 


» Chemical 
Weapons 


» Pharmaceuticals 


» Pesticides 


» Precursors 


» Lab Skills 


» Lab Equipment 


» Safety 


» Roque Science 


» Links 


» What's New 


» Contact Me 


» Disclaimer 


» Search this site 







This list of links contains some of the more useful and informative 
websites that I have found in my web travels. This is not meant to be 
a comprehensive or even useful list, just a starting point for further 
research. I don't necessarily use or endorse all of these links, but they 
are valuable in their own way. If you know of a website that you think 
fits within one of the categories here, just email me and I will check it 
out. 



Labware Links 

Advance Scientific Mid-sized company that provides reasonable selection of lab equipment 
and some chemicals, a bit pricey in my opinion. This company is rumored to be a front for 
DEA sting operations, so buy chemicals from here at your own risk. Chemical sales are 
restricted to companies and universities only. Printed catalog is $5.00, they do not offer 
online shopping. 

BLWA The Association of the Laboratory Supply Industry. A UK based directory of over 
160 European laboratory supply companies. 

Chemglass A manufacturer and supplier of Standard Taper glassware with reasonable prices. 
They offer a free printed catalog. 



http://www.roguesci.org/megalomania/links.html (1 of 3)12-8-2004 17:22:57 




Megalomania's Link Section 



Corning Lab ware & Equipment Corning is one of the largest manufacturers of lab glass, but 
you must order through a company as they do not sell direct except to dealers. The website 
offers a complete catalog and an index of authorized distributors. Print catalogs are available. 

Daigger Offers good selection of lab equipment at reasonable prices. They offer a free 
printed catalog or online shopping. 

Fisher Scientific A large supplier of lab equipment, but with high prices in small quantities. 
Average selection of overpriced chemicals, restricted to companies and universities only. 
They offer a huge free printed catalog and online shopping. 

Indigo Instruments Offers limited selection of lab equipment priced well for small quantities. 
They mainly sell unusual items for school science labs. 

Lab Depot Offers an apparently limited selection of lab equipment and chemicals on the 
website, but they say they have lots. They also say they sell to individuals. They offer a free 
printed catalog or online shopping. 

Lab An online auction website selling new, used, and refurbished lab equipment from 
many different companies and individuals. This is a very unique place where good deals can 
be had on used equipment or in the auction. 

Thomas Scientific Offers a large selection of name brand scientific supplies for industry 
only. Free catalog available to scientists only. 

Voigt Global An international supplier of lab equipment and chemicals. They are scared to 
death of selling any drug precursor, so they do not sell many basic chemicals. No prices are 
offered online, nor is there a print catalog that I am aware of. 

One of the largest suppliers of lab equipment, but very very expensive in small 
quantities. Average selection of overpriced chemicals, restricted to companies and 
universities only. They offer a huge free printed catalog or online shopping. 

Chemical Suppliers 
Other Science Links 
Explosive Sites 

Aerodynamic Inventions A very informative website about pneumatics and pyrotechnics 

Bruce's Bombs, Explosives, and Ordinance Page General explosives information geared 
towards safety and law enforcement types 
DaveBoomlndex A small list of links related to explosives 

Explosives & Pyrotechnics Information Database A good page, but its creator is a difficult 
person to get along with 



http://www.roguesci.org/megalomania/links.html (2 of 3)12-8-2004 17:22:57 



Megalomania's Link Section 



Vaeyens Senne's explosives thesis An academically written site with general explosives data 

Political Links 
Chemical Weapons 

Introduction to Chemical Warfare A brief overview of the use of chemical weapons, nothing 
of true value 

Biological Weapons 
Nuclear Weapons 



Drugs 



The Hive This is a great discussion board for all matters of drug synthesis and chemical 
acquisition. Read all you can before posting because they do not tolerate the ignorant. This 
site was the primary inspiration for me in creating my explosives forum. 

Lycaeum This is one of the largest and best sites for information on recreational drugs and 
for drug synthesis. It is a huge and comprehensive database on all things drug related. 
Rhodium One of the top drug synthesis archives. This site has a massive section of synthesis 
procedures for many precursors. It is kind of the drug equivalent of my site. 

Poisons 



Megalomania's Controversial Chem Lab ©1997-2004 /links/ revised January 31, 2004 



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All about Megalomania's Controversial Chem Lab 




Navigation 


» Home 


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» Chemical 
Weapons 


» Pharmaceuticals 


» Pesticides 


» Precursors 


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» Lab Equipment 


» Safety 


» Roque Science 


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» What's New 


» Contact Me 


» Disclaimer 


» Search this site 







Megalomania's Controversial Chem Lab is a web site devoted to 
publishing chemical information on any substance that has been 
deemed "unacceptable" to use, posses, sell, consume, etc. The 
chemicals here are dangerous, yes, but they are also very interesting. 
These substances capture the attention of the news media and the 
general public every day, primarily for there misuse. 

I wanted to create a place where those with little scientific skill 
could learn the trade while being informed about chemistries hidden 
side. Within this web site are methods of synthesizing a variety of 
chemical compounds including explosives, drugs, poisons, medicinal 
compounds, and chemical weapons. There is also extensive 
supporting information to assist you in understanding these labs. I 
have made sections on laboratory safety, explanations of laboratory 
equipment, skills and terms used in all these labs, and a more or less 
comprehensive section detailing how every precursor chemical used in 
the sites labs can be synthesized themselves. 

What I do not provide are any means of building detonators, 
bombs, delivery systems, or any other means of actually using these 
chemicals. This information could facilitate a misuse of these 
compounds for criminal purposes. These labs are provided for 
educational purposes only. 

I have gone to great lengths to include more than the average 
amount of information on preparing a chemical. No where else can 
you find links within the Lab directing you to the chemicals used, or 
the equipment needed, or even an explanation of this or that Lab 
skill. I hope that someday the chemical preparations here will become 
incidental to the safety information, the explanations of laboratory 
equipment, the definitions of chemistry terms, and the clear 
explanations on how to perform a Lab technique. 



The update history: Progress and direction. 



Projected Status for 2002: 

I have decided to refocus back on explosives again. All of the precursors and the other areas still need a 
lot of work, but explosives are what I do best, so I want to offer more. Specifically I will be researching 
the latest and greatest 21st century explosives fresh from the lab, with some older mid 20th century stuff 
thrown in. I may also begin to get my own precursor research underway. I have already started 
experiments on homemade nitric acid, and my theory on making benzene is very solid now. I also plan a 
few molten electrolysis experiments. 



http://www.roguesci.org/megalomaniaywhatnext.html fl of 7)12-8-2004 17:22:58 




All about Megalomania's Controversial Chem Lab 



Status as of February 10, 2002: 

As you may well be able to tell, the rest of 2001 was not a banner year. I have devoted my time almost 
exclusively to The Explosives and Weapons Forum. I have not taken the time to find any new explosive 
or precursor information, nor have I really conducted any experiments. I am truly sorry for that, but that 
is all behind me now. Needless to say this is less of an update and more of a status report, since I have 
nothing new to add but news. My site was finally deleted from Internettrash after some 2.5 years, they 
are now completly defunct, offering no new signups, no tech support and their systems shut down more 
and more. The past year has seen the bottom fall out of the Internet market, and with it all the free stuff. 
Free providers are still a dime a dozen, so I will find another. I guess it is time for my own domain. 

Status as of May 1, 2001: 

Well, the past 7 months have seen some significant changes. Since my last update I have been steadily 
adding more information to the synthesis section. Unfortunately I have not taken the occasion to update 
the site. Of course I had my usual slump of not doing anything for some periods of time and doing lots 
in a short time. The past few months I completely rearranged the look of the site. I changed the color 
scheme, removed some graphics, and added some of my own. I also changed the name of the site. The 
changes are to lend an air of professionalism that I think the old site did not carry across. The new site is 
more efficient and less likely to be associated with some "kewl" anarchy page. 

Status as of October 1, 2000: 

Wow, it has been a long time since I have done an update, yet I have done so much in the past 5 months. 
I have delved into the synthesis section with full force, and it is indeed a daunting task. There are about 
170 different chemicals in the synth section, I found about 90 synths in my search so far. I actually 
added a dozen or so, I even found some synths for the synths. I see a disturbing trend, for each chemical 
I find a synth for, I will need an average of 2 new chems to add to the synthesis section. Fortunatly, for 
every synth of a synth I find I only need 1 chem per 5. Still that means it will take me years. I finished 
adding all the physical constant data, I made a huge synonym index that too me a long long time to do, 
and I have added in a few of my synth writeups. The writeups are not actually linked or anything yet. I'm 
sure I did alot more I forgot about. 

Status as of May 1, 2000: 

A long 3 months have passed with nothing done to the site, after the Great Edit I decided to take a break 
and work on other projects. During the month of April I returned to the site in earnest and began work 
on the synthesis section. Indeed, numerous edits to every explosive Lab have been made because of 
changes to the synth section. I changed the table format of the chemicals, standardized the names of the 
chemicals to eliminate duplicates, and began to add some much needed physical and safety data. If you 
want actual synthesis info you will have to wait a bit longer. Unfortunately my estimates put completion 
of the synthesis section sometime around 2002! This project is very daunting and comprehensive, but no 
other website has anything similar. The chemicals will be added throughout the next 2 years, not in 
suddenly in 2002 in case you are worried. I will update the zip archive next month. 



http://www.roguesci.org/megalomania/whatnext.html (2 of 7)12-8-2004 17:22:58 




All about Megalomania's Controversial Chem Lab 



Status as of January 15, 2000: 

After finishing the "minor update", and after working so hard the previous month, I have completly 
slacked off. Only the first few days of December saw any changes, I skipped the new years update, now 
here it is. Basicially this update is a brand new equipment section with updates to all pages to reflect a 
change in links. I also updated the zip archive. 

Status as of December 1, 1999: 

This past month has been very industrious. I have delved into the "minor update" with enough 
enthusiasm to complete numerous changes on every page. No technical information was added, the 
update is solely devoted to improving the aesthetic quality of the site. A large number of bad links, 
missing pages, and erroneous anchors were discovered and fixed. There were so many changes I even 
did an update on Nov 16. 

Status as of November 5, 1999: 

The Great Edit is finally done! After so many months devoting most of my time working on this, it is 
good to be done. Progress on the website will continue, though. My computer has been buggy for most 
of the late summer, in early October I finally deleted the hard drive, re-installed Windows 98, and set the 
computer up with all new software. These problems were what considerably slowed my working on the 
site. Now I am doing a project called the "minor update." The update will focus on details, making sure 
all the links go where they should, shuffling around the directories, and basically making the site more 
functional. I have actually done changes to so many pages the first few days of November that I have 
delayed the upload from the first to the fifth. 

Status as of September 14, 1999: 

A large number of computer problems, made all the worse by the disappearance of my Windows CD, 
have plagued me for a month. Other demands on my time have cause me to neglect updates and working 
on the site. The accursed Great Edit is still not done, but I am very close, very close. I did get many labs 
done surprisingly, I had just hoped to be done by now. 

Status as of July 5, 1999: 

Since the July 1 update was a disaster, I have done it again. The FTP for nettrash was buggy, it cut out a 
few hundred bytes from every html file. The archive should be updated as well. 

Status as of July 1, 1999: 

I think I made some progress on the Great Edit this month, the end is now in the foreseeable future with 
over 70% of the edit done. There is no reason why I can not be done by the August update. I mean it this 
time. I decided to do a preemptive strike this month and move my site to a new home at www.nettrash. 
corn instead of waiting to be deleted from Xoom. The people at nettrash are very sympathetic to a site 
like mine. The only drawbacks so far are the 10MB size limit which will hinder future expansion, and a 
sketchy FTP upload which to get I had to sell my soul to the pop-up ad devil. Since my site has yet to 
reach 10MB there is no problem yet, I suspect they will give more in the future. The search engine 
should be working again, Xoom inserted some damn redirect code that made it impossible to scan the 



http://www.roguesci.org/megalomaniaywhatnext.htmI (3 of 7)12-8-2004 17:22:58 



All about Megalomania's Controversial Chem Lab 



site. Other than some minor editing changes and a change to the nav-bar again, that's about it. 

Status as of June 1, 1999: 

I have decided to divide some of the time spent on the Great Edit to work on the synthesis and 
techniques section. Gee, that sounds like last month, but this month I actually did stuff, although not 
much. It has taken me 5 months to get halfway done with the Edit, it would have taken a more dedicated 
person a month. I got taken down , again, from Fortunecity, I now reside at Xoom once more. I have 
been working on a plan to reside at a large number of web servers, censors beware. I now have a site that 
likes pages like mine, if Xoom doesn't like me then I will be up and running in minutes at my new home. 
I have also unraveled a conspiracy. It seems my page does not appear on any search engine, I wonder if 
someone is out to get me. It is possible they just updated their links and booted my pre-surf.to address, 
but with all the nonexistent crap that they keep, it is unlikely. It doesn't matter to me if I drop out of the 
public eye for a month or a year. I will keep on building this site and then spring it on ya. I will submit 
my site to so many search engines that nobody could get rid of me. 

Status as of May 1, 1999: 

Working on the Great Edit has been slower than I expected. I have decided to throw in a mixture of 
chemical synthesis, and techniques data instead of just concentrating on the Edit. Of course, I did not 
actually add any. I did add a search engine to search only this site, that should come in handy. 

Status as of April 1, 1999: 

Even though I have largely skipped a March update, I did have to do an emergency update during the 
middle of February when fortunecity had their computers crash and lost many web pages. I have been 
thinking of not doing an update until I get the Great Edit done, but there is no need to withhold any 
information from the public. I would like to say that in the 3 months since I started the Great Edit I 
would have more done. Sadly, I estimate approximately one third of all the labs are done. Now I hope 
this does not mean by September 1st I will be all done! I want to make April the last month of the Great 
Edit so I can move on to other areas of improvement and begin to add more information instead of all 
this double checking. 

Status as of February 1, 1999: 

I spent the first half of the month making editing changes on paper and I put several on the web, then it 
seems I slacked off a bit. 

Status as of January 1, 1999: 

Actually, it’s December 31. Due to illness, my computer usage was sporadic. Thus, I did not accomplish 
much in December. I did, however, make many changes on paper, just not online. What I did do was put 
the synthesis and equipment pages and graphics into their own folders. This necessitated all pages have 
the nav bar fixed as well. I also discovered a slandering censor, onno601 @ mailcity.com , is the 
responsible party for removing my page from xoom. Please email him lengthy letters describing how 
evil and wrong his actions were. Email often. To insure that I can not be defeated by Nazi book burners 
like ohno, I have changed my site to http://surf.to/megalomania . A redirect site that will always point to 



http://www.roguesci.org/megalomaniaywhatnext.htmI (4 of 7)12-8-2004 17:22:58 



All about Megalomania's Controversial Chem Lab 



my page no matter where it may reside. 

Status as of December 1, 1998: 

Early this month I completed listing the chemicals in the tables of the explosive labs, and I filled in the 
proper links for the next/previous link at the bottom of those pages, next on the agenda was going 
through each Lab and adding any chemical on the table to its own table on the synthesis pages. At this 
point the synthesis pages were so huge I split them into 5 parts in anticipation of adding the synthesis 
data. To make matters worse my xoom site has mysteriously disappeared, it is now at fortunecity. The 
only problem I have with fortunecity is that darned banner they put on top of each page. 

Status as of November 1, 1998: 

This month has actually been rather non-industrious. I took some weeks off, all I really accomplished 
was filling in the chemicals used into the table of several explosives labs. 

Status as of October 1, 1998: 

This month has actually been rather industrious. I have started to revise all of the explosive labs and link 
them to the other sections. I did a major overhaul on the nav-bar and other minor code changes to all 
pages. A few more months like this and I may get done. HAHAAHAH, I crack me up. The message 
board mysteriously disappeared so it needed replaced, and I uploaded the entire site once again to be rid 
of some file renaming gremlins. 

Status as of September 1, 1998: 

I almost completed every one of the explosive labs, but still not quite and then there only in raw form. 
Perhaps this month will be better as I start to make what I have better. 

Status as of August 1, 1998: 

Well, July is at a close and what have I got to show for it eh? I removed the pages from the web site 
because I needed to revise all the file names and get everything synchronized. Furthermore, the lack of 
support pages like safety and techniques and other aspects of the web site make it seem, well, blah. To 
top it all off the computer was stricken with a case of spiteful rage when "somebody" screwed up my 
CMOS and set the damn thing to write protect. After two weeks in the shop its fine, but that just blew 
most of July. Combine that with my typical apathy and laziness during the summer and even less work 
got done. Most of the work done has been minor editing changes. 

Status as of July 1, 1998: 

Darn it, I made this update on July 1st, but it seems I have lost my older page so now I am writing this 
on August 1st... nothing happened anyway during the rest of June except that I worked on getting more 
explosive labs done. 

Status as of June 1, 1998: 

Wow it seems that I haven't done an update for awhile! OK, OK, let me see, some time ago I had been 
removed from my web site at geoshitties for copyright violations because I linked to a site only 



http://www.roguesci.org/megalomania/whatnext.html (5 of 7)12-8-2004 17:22:58 




All about Megalomania's Controversial Chem Lab 



temporarily to test some graphics, that was back in February I suppose. Now I have some more but I 
have made the decision not to put up the site until I at least get most of the information done. Oh boy 
and how much there is to do though. I have been working on this site on and off, mostly off, for nearly a 
year now and I still don't have it nearly done. Every time I get something done I decide I need to add 
more, ick. Just putting the explosives info up alone is a task and a half, let alone the safety, equipment, 
techniques, synthesis, and other sections. I have acquired many new explosive information only in April, 
I must have added 20 more, there is still more to be found, and of the ones I have, they need to be made 
into pages. Sigh... guess I will see ya next year :) 

Status as of December 18, 1997: 

Well it seems I finally got my synthesis page the way I want it to look template wise and fixed a big 
problem with the pesky table alignment. I have all the pictures for Lab equipment I want now so I can 
start on that and I finally filled in the last explosive (TNT) so those are basically done until I edit them 
all again, they need typo checked and accuracy double checked. Now I will go back through all the labs 
and add in the anchor links to the synthesis section and Lab equipment. After that I will start filling in 
info for those pages. Still a lot more to go. 

Status as of December 11, 1997: 

All rightly, I have been somewhat lazy after that crash way back when and now I have reached an 
impasse. I have tinkered somewhat with the pages but I have been unsure how to proceed on the 
synthesis section. I need to start doing that page so I can add in the anchor links from the explosives 
pages. I have found a stash of pics for the equipment and some procedures but that comes after the 
synthesis stuff. As you may have noticed all the explosives still need editing for the final way they will 
look (with formulas, class, weights, etc.). I also need to rewrite many of them because they are supposed 
to provide info that normally would be provided in the synthesis section. It seems like the more I get 
done the more I decide to do... I also don't have a computer anymore and have to use the public libraries 
( soon (January) I will be back in college and will have a much better computer Lab to use all I want. 

Status as of August 20, 1997: 

ACK! On July 20 my hard drive crashed and had to be taken to the shop. It work a few days on August 
3-5 then it was back to the shop. Only yesterday did It work. That's a slight delay to getting things done 
around here. 

Ok here is the status of the site as of July 18, 1997: 

I finally finished making the template of how the pages will look using my new Hotdog program, which 
just crashed yesterday, so that's been my biggest hurdle. Now I have started to bring out all the scientific 
info I have been collecting on explosives for the last several years. The editing has begun, I finished the 
acetone peroxide somewhat and am now on the NI 3 part. Maybe I will be done by September with all 
these procedures. I just got selected as a demo tester for Cambridge Soft's ChemDraw, so my search for 
a molecular modeling program is finally at an end. Well that's about all for July 18. 

In the Beginning: The origin of Megalomania's Controversial Chem Lab. 



http://www.roguesci.org/megalomania/whatnext.html (6 of 7)12-8-2004 17:22:58 




All about Megalomania's Controversial Chem Lab 



Megalomania's Explosives and Stuff owes its beginnings to my long love of chemistry and 
explosives. When I was a young child and teen, I purchased several tomes of wisdom of an anarchist 
nature. These improvised explosive books were appallingly simple and poorly written crap. I was 
stunned that somebody could write a book and still not say anything, worse yet I had spent my precious 
money on a scam. The thought briefly flickered in my head that even I could do better. 

It was not until my college years that I began the serious undertaking of finding the laboratory 
methods of synthesizing explosive compounds. I wrote as many as I could find in a work I called "The 
Paper." While researching the information, and reviewing the labs, I realized that every one had some 
outlandish and unobtainable precursor. This led me to research how the precursors themselves are made, 
and "Project Progenitor" was born. All of this information was solely for my own benefit, I wanted to 
learn this information for my own experiments. I realized that there might be others who would benefit 
from my research so I hatched a plot to use the university printers to make pamphlets. Pamphlet one for 
explosives, pamphlet two for precursors. The idea did not pan out though, I had no real means of 
distributing the information other than dropping them around campus. 

College was also the start of my using a computer, a real computer, not just an outdated PC using 
BASIC. I got my start on a Mac, then I discovered Windows and, most importantly, the Internet. I 
seemed to grasp the concepts of using the Internet quickly. I realized it could be a great tool for mining 
information, so I set out to surf for explosive sites. All crap, there was this thing called the Jolly Rogers 
Cookbook and the Anarchists Cookbook, pure drivel then and still sought by fools today. No real 
information. I had no idea what HTML was or how to get a web page. Then I got a computer science 
major as a roommate, I learned a lot, still no HTML however. 

It was a year later when I left the university that I thought "why don't I make a web page?" So, I 
searched for HTML help and free webspace and found a nice page that I used as a template. The name 
Megalomania is one I used a lot on computer games, everybody needs a handle, so I made it 
Megalomania's Explosives and Stuff, a catchy and humorous title. The first incarnation of the site was 
March 12, 1997. 1 used all the information I had from "The Paper" and "Project Progenitor" to flesh out 
the explosives and synthesis sections. I realized that writing for a laymen audience needed something 
more. I like to create where others leave off, I wanted a page that if I knew nothing about explosives, I 
would learn here. 



Megalomania's Controversial Chem Lab ©1997-2004 /whats new/ revised January 31, 2004 



http://www.roguesci.org/megalomania/whatnext.html (7 of 7)12- 



■2004 17:22:58 




The disclaimer 












DISCLAIMER!! 



All of the procedures contained herein are potentially hazardous to life, limb, and 
property, as is any application of chemistry. Under no circumstances are you to actually 
follow any of these instructions without proper authorization or scientific training. This 
website is intended to provide information only. An unskilled individual should never 
attempt any of these procedures. No guarantee is given or implied regarding the 
accuracy of the contents. The author can not be held responsible or liable for the use or 
misuse of the contents of these documents. Sections have been provided for proper 
laboratory procedures, chemical handling, laboratory safety, and other essential 
information, so that other aspects of chemistry can be learned and used. It is necessary 
to have a licence from the US government to manufacture, posses, transport, use, 
handle, sell, buy, or experiment with explosive compounds, although they have to give 
you such a license if you apply and meet the requirements. The same applies to chemical 
weapons, most pharmaceuticals, and some pesticides. It is your responsibility to comply 
with the law in your own region or country. 

By viewing this site, you understand and affirm that: 

1. You will not use, or allow to be used, the information contained herein in a manner 
injurious or damaging to any person, animal or property. 

2. You will not use, or allow to be used, the information contained herein in a manner 
which is an infraction of any laws applicable to the place in which you live. 

3. You do not support terrorism or crime in any manner. 

4. The author and publishers are not responsible or liable to anyone for the use or 
misuse of the information contained herein. 

5. You will not use, or allow to be used, the information contained herein to aid the 
illegial manufacture or use of explosives or explosive devices. 

6. Any person using the information in these documents does so entirely at their own 
risk and in violation of this agreement. That person bears sole responsibility and 
liability for any claims or actions, legal or civil, arising from such use. 

7. You will not give, transmit or divulge any information contained herein to any third 
party or recipient without that third party reading, understanding and affirming to 
this disclaimer. 

8. You will not make or transmit any copies of any information contained herein in 
any form, including but not limited to: Copies held on computer storage media, 
print-outs, photocopies, facsimiles, photographs and written copies. 



http://www.roguesci.org/megalomania/disclaimer.html (1 of 2)12-8-2004 17:23:00 



The disclaimer 



9. No action will be taken against the author or publishers on the grounds that these 
documents infringe anyone's copyright. If you believe these documents to be in 
breach of anyone's copyright you will inform the author immediately so the 
offending material can be removed upon receipt of proof of copyright for that 
material. 

10. The author is not responsible for the storage or accessibility of these documents on 
any system in a place where such storage or accessibility infringes local law. If 
such a situation exists, it is the responsibility of the owner of said system to comply 
with the law. 

11. No criminal or civil offence is being committed by accessing or reading these 
documents. 

12. By allowing these pages to be uploaded, the space provider of Megalomania's 
Controversial Chem Lab agrees to exempt this site, its author, and any other agent 
involved in the sites creation, from any terms of service past, present, and future. 
Furthermore, the space provider agrees to be held only to the terms of service 
listed by this disclaimer, and to abide by any future policy changes and mandates. 
The space provider agrees to not delete this site and to be held solely legally 
accountable for any violation this site may incur. 

A note on copyrights: The original scientific and technical information on this web site 
is not protected under copyright law, all information from copyrighted texts has been 
reproduced with respect to the "fair use" clause of U.S.C. Title 17. All graphics and 
sounds not original creations of the author are freely distributable as long as they are not 
modified. All other graphics and text are copyrighted by the author and may not be 
copied, modified, displayed, or otherwise misused unless prior written consent is obtained 
from the author of this web site. The use of any information, lab, or graphic from this site 
will probably be granted as long as a link is provided from the users page to this website, 
http://surf.to/meqalomania and an email is sent to me at meqalomania(5)scientificmind. 
com describing what was taken and where it is on the users site, as well as the users 
homepage. 

Megalomania's Controversial Chem Lab ©1997-2004. 

Home j Explosives i Chemical Weapons : Pharmaceuticals ] Pesticides ! Precursors 
Lab Skills ' Lab Equipment ! Safety ! Roque Science : Links ! What's New | Contact Me l Disclaimer 



Megalomania's Controversial Chem Lab ©1997-2004 /disclaimer/ revised January 31, 2004 



http://www.roguesci.org/megalomania/disclaimer.html (2 of 2)12-8-2004 17:23:00 




Glassware 



Glassware 




Adapters 

What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 




Beakers 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



2 





http://www.roguesci.org/megalomania/equip/glassware.html (1 of 10)12-8-2004 17:23:43 




Glassware 




Bottles 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Bubblers 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/glassware.html (2 of 10)12-8-2004 17:23:43 






Glassware 






Burets 


What It Is: Blah, Blah, Blah, Blah 


Where To Get It: Blah, Blah, Blah, Blah 








Condensers 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/glassware.html (3 of 10)12-8-2004 17:23:43 





Glassware 




Crucibles 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 





Dishes 

What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/glassware.html (4 of 10)12-8-2004 17:23:43 






Glassware 




’VP 

H/ 

I 



Distilling Columns 

What It Is: Blah, Blah, Blah, Blah 

Where To Get It: Blah, Blah, Blah, Blah 





Drying Tubes 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/glassware.html (5 of 10)12-8-2004 17:23:43 







Glassware 




What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/glassware.html (6 of 10)12-8-2004 17:23:43 





Glassware 




Funnels 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 





Graduated Cylinder 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 



Mortar and Pestle 



What It Is: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/glassware.html (7 of 10)12-8-2004 17:23:43 





Glassware 







Pipets 


What It Is: Blah, Blah, Blah, Blah 


Where To Get It: Blah, Blah, Blah, Blah 









Stirring Rods 








What It Is: Blah, Blah, Blah, Blah 




Where To Get It: Blah, Blah, Blah, 
Blah 





http://www.roguesci.org/megalomania/equip/glassware.html (8 of 10)12-8-2004 17:23:43 







Glassware 



I 



Test Tubes 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Tubing 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Watch Glass 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 



Home | Explosives l Chemical Weapons ] Pharmaceuticals l Pesticides ] Precursors 
Lab Skills | Lab Equipment ! Safety | Roque Science | Links | What's New | Contact Me | Disclaimer 



http://www.roguesci.org/megalomania/equip/glassware.html (9 of 10)12-8-2004 17:23:43 



Glassware 



Megalomania's Controversial Chem Lab ©1997-2004 /glassware/ revised January 31, 2004 



http://www.roguesci.org/megalomania/equip/glassware.html (10 of 10)12-8-2004 17:23:43 




Glassware 



Apparatus 




Apron 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Aspirator 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 





Brushes 



http://www.roguesci.org/megalomania/equip/apparatus.html (1 of 9)12-8-2004 17:24:07 






Glassware 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 




Burners 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 



talon clamp 



1 



Keck clamps 5 






http://www.roguesci.org/megalomania/equip/apparatus.html (2 of 9)12-8-2004 17:24:07 





Glassware 




Clamps 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 

















W* ' 1 

V * v 

r * *1 

Hk' . A 

■' — "^^Bi 

*-■ ™ ■*“ ^B 

L - / - 




an economical desiccator 1 


standard desiccator 2 


vacuum desiccator 3 
















Desiccators 


What It Is: Blah, Blah, Blah, Blah 


Where To Get It: Blah, Blah, Blah, Blah 




Filter Paper 



What It Is: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/apparatus.html (3 of 9)12-8-2004 17:24:07 



Glassware 




Gloves 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 




Goggles 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 



Hotplate 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




http://www.roguesci.org/megalomania/equip/apparatus.html (4 of 9)12-8-2004 17:24:07 



Glassware 




Magnetic Stirrer 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




pH Paper 

What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/apparatus.html (5 of 9)12-8-2004 17:24:07 





Glassware 




Pipet Bulbs 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Pipestem Triangle 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 



http://www.roguesci.org/megalomania/equip/apparatus.html (6 of 9)12-8-2004 17:24:07 




Glassware 




% 

r- _M 

e 

V 





Rings 


What It Is: Blah, Blah, Blah, Blah 


Where To Get It: Blah, Blah, Blah, Blah 








Stoppers 


What It Is: Blah, Blah, Blah, Blah 





http://www.roguesci.org/megalomania/equip/apparatus.html (7 of 9)12-8-2004 17:24:07 





Glassware 




Test Tube Clamp 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 






Test Tube Rack 


What It Is: Blah, Blah, Blah, Blah 


Where To Get It: Blah, Blah, Blah, Blah 






' ^ — — 


Thermometer 


What It Is: Blah, Blah, Blah, Blah 


Where To Get It: Blah, Blah, Blah, Blah 




http://www.roguesci.org/megalomania/equip/apparatus.html (8 of 9)12-8-2004 17:24:07 






Glassware 




Tongs 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Tubing 



What It Is: Blah, Blah, Blah, Blah 



Where To Get It: Blah, Blah, Blah, Blah 




Wash Bottle 



What It Is: Blah, Blah, Blah, Blah 
Where To Get It: Blah, Blah, Blah, Blah 



Home | Explosives | Chemical Weapons | Pharmaceuticals | Pesticides | Precursors 
Lab Skills | Lab Equipment ! 5afety | Roque Science | Links | What's New | Contact Me | Disclaimer 

Megalomania's Controversial Chem Lab ©1997-2004 /apparatus/ revised January 31, 2004 



http://www.roguesci.org/megalomania/equip/apparatus.html (9 of 9)12-8-2004 17:24:07 




Megalomania's Technique of Distillation 




Distillation 



Distillation is a process in which a liquid is vaporized to a gas, recondensed to a liquid, 
and collected in a receiver. The liquid which has not vaporized is called the residue, and the 
liquid which is collected in the receiver is called the distillate. Distillation is used to purify 
liquids and to separate one liquid from another. It is based on a chemicals volatility, or the 
relative ease of which the molecules leave the surface of a liquid. Every chemical has a 
unique volatility, usually a more volatile chemical has a lower boiling point. The successful 
application of distillation techniques depends on several factors. These include the difference 
in boiling points of chemicals present, the size of the sample being distilled vs. the size and 
type of distillation apparatus, the occurrence of azeotrope formation, and the care you 
exercise. 

You may think that boiling a liquid will release the lower boiling compound first. In 
reality a mixture of the chemicals being distilled will vaporize. There will be more of the 
lower boiling chemical, but, depending on how close each chemicals boiling point are to one 
another, and the ratio of their volumes, the exact compositions will vary. In general, the 
earlier portion of a distillation will be higher in the lower boiling component. As the volume 
of that material becomes less and less, more and more higher boiling component will be 
distilled over. When the boiling points of the chemicals are very close, it is difficult to 
separate them. Sometimes two or more chemicals will form an azeotrope, or a constant 
boiling mixture that can not be separated which has its own unique boiling point different 
from its components. A common azeotrope is ethyl alcohol and water, distillation can only 
get around 95% alcohol and 5% water at best. 

Since not all chemicals distill the same way, there are several distillation techniques that 
are used. These include simple distillation, fractional distillation, steam distillation, and 
vacuum distillation. Some important things to remember for all distillations: Do not fill a 
distilling flask more two-thirds of the way, and never distill a flask to dryness because 
explosive peroxides tend to form and are concentrated enough to blow a flask to pieces. 

Also, you may want to use a boiling stone to prevent bumping, that is a sudden gushing of 
liquid that rushes upwards and may splash out of the flask in simple distillations and hinder 
fractional distillations. A boiling stone is a small piece of marble gravel. 

Simple Distillation 



http://www.roguesci.org/megalomania/tech/distillation.html (1 of 3)12-8-2004 17:24:08 



Megalomania's Technique of Distillation 






A simple distillation is for purifying liquids of one component (separating a liquid 
from solid contaminants), multiple liquids where the differences in boiling points is very 
large (a low boiling liquid from a high boiling liquid), or where time is at a minimum. 
Simple distillations are not effective in removing multiple solvents from one another with 
a high degree of success. 

Assemble the glassware as pictured in figure 1. The picture shows standard taper 
glassware which is superior to ordinary glassware. Ordinary glassware can be substituted 
for standard taper equipment. There should be a clamp on the distilling flask neck, the 
right angle adapter neck, the middle of the condenser, and the receiving flask neck. You 
may need a separate stand for the condenser/receiver clamps. 

Before connecting the distilling flask, add 1 or 2 boiling stones and, of course, the 
materials to be distilled. Adjust the depth of the thermometer so that the bulb is slightly 
below the sidearm leading into the condenser, this is to measure the temperature of the 
vapor, not the liquid in the distilling flask. If you are using ordinary equipment, use a 
short length of glass tubing bent at a 45° angle with rubber or cork stoppers large enough 
to fit into the distilling flask and the ordinary. The stopper in the distilling flask should be 
a 2-hole, a thermometer fits into the other hole. The condenser should be angled 
downward and the thermometer bulb should be just below the bottom of the stopper. The 
glassware on the end of the condenser (drip adapter) that leads into the receiver is not 
really necessary, it is just convenient. The vacuum adapter doubles as a drip adapter for 
standard taper glassware. A drip adapter can be purchased or a length of angled glass 
tubing can be stoppered from the condenser to the receiver. Sometimes hot distillate will 
escape if no drip adapter is used, omit at your own risk. The receiver can be a beaker, 
graduated cylinder, flask, etc. 

Make sure all connections are tight and firm, the clamps tend to pull apart the 
connections as they are assembled. The water inlet of the condenser is always the lower 
nipple (closer to the receiver), the outlet is at the top (closer to the distilling flask). The 
outlet should be pointing up so the water is forced to completely fill the jacket. Double 
check that everything is clamped securely and that coolant water is circulating through 
the condenser. Do not have the water pressure so high that the hose pops off. 

Begin heating the distilling flask until boiling begins. Adjust the heat level so that 
amount of distillate is a steady 2 or 3 drops per second. Discard the first several drops as 
they may have contaminants. Continue distilling until only a small residue remains, not to 
dryness, if distilling pure liquids. When distilling mixtures, the more volatile component 
will be collected in greater concentration at first. As the distillation proceeds a greater 
percentage of the less volatile component will be collected. It may help to change the 
receiver several times to collect different fractions. These separate fractions may then be 
redistilled to collect even purer fractions of each component. Fractional distillations 
handle this task far more efficiently. 




U 



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Megalomania's Technique of Distillation 

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http://www.roguesci.org/megalomania/tech/distillation.html (3 of 3)12-8-2004 17:24:08 



Megalomania's Technique of Filtration 




Filtration 



All about filtration 






Filtration 


How to Filter 




<s> 




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http://www.roguesci.org/megalomania/tech/filtration.htmll2-8-2004 17:24:09 



Megalomania's Technique of Refluxing 





Refluxing 



All about refluxing 



refluxing 




How to reflux 



© 




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egalomania’s Controversial Chem Lab ©1997-2004 /refluxing/ revised January 31, 2004 






http://www.roguesci.org/megalomania/tech/refluxing.htmll2-8-2004 17:24:09 



Megalomania's Precursor Section Part 2 




Precursors Part 2 



A 




charcoal 


C 


1 


mp ? bp ? d ? 


m 12.01115 


c $?.?? 


Safety Data: Flammable 




LABGUARD* 
Storage Code 



C 



A 



Synonyms: carbon ; activated carbon; activated carbon, decolorizing; activated charcoal; animal 
charcoal; carbon, activated; carbon, activated or decolorizing; carbon, amorphous; carbon black; 
carbon decolorizing; carboraffin; carborafine; charcoal, activated 



Synthesis: Coming soon! 



chlorine 



1 



mp -101.00 bp -34.05 







d? 



Safety Data: 



MWl 



Ch 



m 70.906 



1 



c $?.?? 



LAJBGUARD* 
Storage Code 



BLUE 



Cl Cl 



Synonyms: chlorinated water; dichlorine; molecular chlorine 



http://www.roguesci.org/megalomania/synth/synthesis2.html (1 of 20)12-8-2004 17:24:16 





Megalomania's Precursor Section Part 2 



Synthesis: Chlorine gas can be generated in several ways using a wide variety of chemical 

reagents. The amount of material to use will depend on how much chlorine you need, generating 
chlorine does not need precise quantities. The reactants are mixed in such a ratio that keeps the gas 
flowing. 

The most convenient OTC method is the reaction of bleach with Sani-Flush brand toilet bowl 
cleaner. Technically the reaction is between sodium hypochlorite in the bleach and sodium bisulfate 
in the Sani-Flush. The advantage of this is that both are available as OTC chemicals from the 
supermarket. Add a quantity of Sani-Flush to a large Erlenmeyer flask. A one-holed stopper with a 
length of glass tubing connected to a rubber hose is used to direct the gas. Pour a small amount of 
bleach over the Sani-Flush and quickly stopper the flask. The reaction will quickly generate chlorine 
in a vigorous reaction. The reaction will soon subside, shake the flask periodically to stimulate the 
reaction. When shaking is no longer effective, add more bleach to start the process again. When 
adding more bleach is no longer effective, add additional Sani-Flush. Continuing in this manner will 
generate a large amount of chlorine. The most efficient way is to fill the flask one third of the way 
with Sani-Flush and add the bleach dropwise with an addition funnel. When enough bleach has been 
added to create a solution, a magnetic stirrer is used to provide agitation. This method will provide a 
constant flow of gas. 

A second method of generating chlorine gas is to fill a flask one third of the way with small 
pieces of manganese dioxide. To this is added concentrated hydrochloric acid in sufficient quantity 
to cover the solid. On heating, a regular current of chlorine is generated. 

Alternately, chlorine can be generated by adding 1 L of hydrochloric acid to 1 80-200 g of 
powdered potassium dichromate and heating on a water bath. 

Chlorine gas must be dried in some preparations. By passing the gas through a wash bottle filled 
with water, any excess hydrochloric acid will be removed (if hydrochloric acid is used to prepare the 
gas). A second wash bottle filled with concentrated sulfuric acid will remove traces of moisture; the 
presence of water is harmful for most uses of chlorine here. 



chloroacetic acid 


C1CH 2 C00H 


1 




mp 61-63 


bp 189 


d 1.580 


m 94.50 


c $?.?? 


□ 



Safety Data: Corrosive, Toxic 



Synonyms: alpha-chloroacetic acid; chloroethanoic acid; MCA; monochloroacetic acid; 
monochloroethanoic acid 



labguard* 
Storage Code 



WHITE 



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Megalomania's Precursor Section Part 2 



Synthesis: Prepare a mixture of 12 g of red phosphorus and 143 mL of glacial acetic ; in a 250- 

mL Florence flask. Connect a Clasien adapter to the flask; attach a reflux condenser to the angled 
arm, and a thermometer adapter to the straight arm. Instead of using a thermometer in the adapter, 
place a piece of glass tubing that extends to the bottom of the liquid. This is an addition tube for 
chlorine gas , using a bubbler on the end of the tube can improve the reaction. 

Locate the apparatus in a location that it can receive as much sunlight as possible, even to the 
point of positioning mirrors to get more sunlight. The sunlight is very important as the light provides 
the photochemical energy necessary for this reaction to succeed. Ordinary lamp light will not work, 
nor will this reaction be very effective during the winter months. The best time is midday during 
summer. With adequate sunlight the reaction will require as little as 12 hours (essentially all day 
while there is light) and in winter it will require two or more days (stopping for the night). The 
longer it takes, the more chlorine that will be wasted. 

While heating the flask on a vigorously boiling water bath, pass a current of dry chlorine gas into 
the acetic acid. The completion of the reaction can be determined by taking a small sample into a 
test tube and cooling it in an ice-water bath. If the sample solidifies after rubbing the walls of the test 
tube with a glass stirring rod, it is done. After the reaction is complete, set the flask up for simple 
distillation. Distill the contents, collecting the portion that distill over from 150 to 200 °C in a 
beaker. Cool the beaker in a salt-ice bath, rub the walls with a glass stirring rod. The portion that 
solidifies, consisting of pure chloroacetic acid, is rapidly suction filtered, the loose crystals are to be 
pressed together with a spatula or spoon to squeeze out excess liquid. The suction must not be 
continued too long because the chloroacetic acid gradually becomes liquid in warm air. The filtrate 
is again distilled, but this time the portion distilling over from 170 to 200 °C is collected in a beaker. 
A second portion of chloroacetic acid is obtained by cooling and filtering as before. The two 
crystalline portions are combined, and then distilled to obtain perfectly pure chloroacetic acid; yield 
can vary from 80-125 g. 

Although this reaction primarily synthesizes chloroacetic acid, some amounts of dichloroacetic 
acid, and trichloroacetic acid will also be made. These can be obtained from the filtrate and what 
does not boil over during the distillations. By continuing the reaction beyond what is necessary to 
make chloroacetic acid, you will eventually end up with mostly trichloroacetic acid. This will take 
several extra days though. The rate of the reaction can be facilitated by the addition of a small 
quantity of iodine to the acetic acid and phosphorus. This will cause some amount of contamination 
(iodoacetic and chloroiodoacetic acids), but a greater yield will be achieved in less time. 

It is possible to substitute sulfur for red phosphorus in this reaction, which is much more readily 
available, but it is not as efficient as phosphorus . It is also possible to conduct this reaction using 
bromine instead of chlorine; bromoacetic acid is thus obtained. Getting iodine products is only 
possible by treating the corresponding bromo or chloro compounds with potassium iodide. 
Furthermore, other carboxylic acids can be used instead of acetic acid, as long as it has an alpha 
hydrogen (a hydrogen atom on the carbon that is bonded to the carboxylic functional group). 











chlorobenzene 


C 6 H 5 C1 


1 


1 



http://www.roguesci.org/megalomania/synth/synthesis2.html (3 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 



mp -45 



bp 131-132 



d 1.107 



m 112.56 



Safety Data: 



MSDS 



Flammable 




Synonyms: benzene chloride; chlorobenzene mono; chlorobenzol; MCB; monochlorobenzene; 
monochlorobenzol; phenyl chloride 

Synthesis: Nothing yet 



chloroform 


CHC1 3 


1 


Cl 

Cl 


mp -63.5 bp 61-62 d 1.484 


m 119.38 


c $?.?? 


Safety Data: MSDS 


LABGUARD' 
Storage Code 

BLUE 




Synonyms: trichloromethane; formyl trichloride; methane trichloride; methenyl trichloride; methyl 
trichloride; R 20 (refrigerant); refrigerant R20; trichloroform 


Synthesis: Coming soon! 




Synonyms: 2-hydroxy- 1,2, 3 -propanetricarboxylic acid; aciletten; citretten; Citro; hydrocerol a; 
hydroxy- 1, 2, 3-propanetricarboxy lie acid; hydroxytricarballylic acid; 2-hydroxytricarballylic acid; 
beta-hydroxytricarballylic acid 



Synthesis: Coming soon! 







copper 


Cu 


1 





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Megalomania's Precursor Section Part 2 



mp 1083 



bp 2595 



d 8.94 



m 63.546 



c $?.?? 



Safety Data: 





LA&GUARD* 
StMyB Code 



Cu 



Synonyms: ANAC 110; arwood copper; CDA 102; CDA 122; C.I. 77400; CuTEA; cutrine-plus; 
komeen; pigment metal 2; Raney copper 



Synthesis: Coming soon! 



ra-cresol 



C 7 H 8 0 



mp 11-12 bp 202 



d 1.034 



m 108.14 



Safety Data: Corrosive, Toxic 




Synonyms: 3-methylphenol; cresol; cresylic acid; cresylol; tricresol 



Synthesis: Prepare a solution of 5.4 g of m-tolylboronic acid and 100 mL of ethyl eth in a 250- 

mL round-bottomed flask. Drop in a magnetic stir bar and attach an addition funnel to the flask. 
While stirring, add 30 mL of 10% hydrogen peroxide from the funnel over a period of 5 minutes. 

The reaction will generate heat as the reaction commences. After all of the peroxide has been added, 
continue stirring until the contents of the flask have cooled to room temperature. This will require 
about 20 to 30 minutes. 

After cooling, transfer the contents to a separatory funnel. Drain off the lower aqueous layer and 
discard it. Wash the remaining ether layer by shaking with three 30 mL portions of 10% mmonium 
ferrous sulfate solution. This removes any remaining peroxide. Again discard the lower aqueous 
layers. Next, extract the product from the ether by shaking with three 30 mL portions of 10% sodium 
hydroxide solution. This time keep and combine the aqueous extracts, discard the ether layer. 

Acidify this solution by adding an excess of concentrated hydrochloric acid , and then extract the 
product by shaking with three 70 mL portions of ether. 

Dry the combined ether extracts by adding several grams of calcium sulfate, shake for a minute, 
and then filter to remove the sulfate. Remove the ether by allowing it to evaporate. Linally, distill the 
crude product to collect pure m-cresol. The yield is 58% or about 2.5 g. 



cupric sulfate 



CuSCk 



http://www.roguesci.org/megalomania/synth/synthesis2.html (5 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 



mp 560 (dec) bp - 

•• 



d 3.6 



m 159.61 



c $?.?? 



Safety Data: M 






LABGUARD* 
Storage Code 

"blue 



X 

Z x 
unknown 



Synonyms: bluestone; blue vitrol; chalcanthite; copper sulfate; dried cupric sulfate; hydrocyanite; 
Roman vitrol; Salzburg vitrol 

Synthesis: Coming soon! 



A 



dextrin ( c 6 H io° 5 )n+ 


1 


X 

Z * 
unknown 


mp - bp - d ? m - 


c $?.?? 


Safety Data: MSDS 


ChemAlcn* 
Sid rage Coda 

GRAY 










Synonyms: British gum; canary dextrin; corn dextrin; dextrin hydrate, white; pyrodextrin; starch 
gum; torrefaction dextrin; white dextrin; yellow dextrin 


Synthesis: Coming soon! 



A 



2,3-diazido- 1 ,4-butanediol 


X a Y b Z c 


1 


X 

J"7 ? > 
z * 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: SDS 


ChemAlcn* 
Sie rage Coda 

GRAY 

fry- 1 * ' : r , iirB 




Synonyms: 


Synthesis: Nothing yet 



3,3-diazido-2,4-pentanediol 



X a Y b Z c 



1 



mp 



bp? 



d? 



m ' 



c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis2.html (6 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 



Safety Data: MSDS 
J 


GhemAlcrO 
Sic ra ge Code 


Ok 4 


GRAY 





Synonyms: 



v 



X 

unknown 



» 



Synthesis: Nothing yet 

■ 



A 



1 ,3-dichloro-2, 4, 6-trinitrobenzene x a Y b z c 


1 


X 

Z * 
unknown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: MSDS 


GhemAleri* 
Sic rage Code 

GRAY 




Synonyms: 


Synthesis: Nothing yet 



A 



dicyanodiamide C 2 H 4 N 4 


1 


NH 

V. A 

tr rn-u 

h 2 


mp 209.5 bp? d 1.400 m 84.08 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl* 
Sic rage Code 

GRAY 




Synonyms: cyano guanidine 1 , 1-cyanoguanidine; 2-cyanoguanidine; DCD; dicyandiamide 


Synthesis: Nothing yet 



A 




A/yV-di methyl aniline 


c 8 h„n 


1 




mp 2 


bp 192-194 


d 0.956 


m 121.18 


c$?.?? 



http://www.roguesci.org/megalomania/synth/synthesis2.html (7 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 




A 



N,N -dimethylformamide 


HCON(CH 3 ) 

2 


1 


X 

Wv 

z 1 

unknown 


mp -61 bp 153 d 0.9445 


m 73.09 


: $?.?? 


Safety Data: Flammable, Toxic 


LAFiGUARD* | 
Corse 


Synonyms: DMF; DMFA 


Synthesis: Nothing yet 



m - dinitrobenzene 


c 6 h 4 n 2 o 4 


1 


X 

Ml 

z 1 

mknown 


mp 89-90 bp 300-303 d ? 


m 168.11 


c $?.?? 


Safety Data: MSDS 


GhemAlerl 1 
Sid rage Code 

GRAY 





Synonyms: 



http://www.roguesci.org/megalomania/synth/synthesis2.html (8 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 



Synthesis: Prepare a mixture of 14 mL of 99-100% sulfuric acid and 10 mL of fuming (+1% to 

+10% free N0 2 ) nitric acid. Slowly add the nitric acid to the sulfuric acid in a 250-mL Erlenmeyer 

flask cooled in a salt-ice bath. After the acid mix has cooled to room temperature remove from the 
cooling bath. Slowly add 8.5 mL of nitrobenzene to the acid in a well ventilated area. The mixture is 
then heated on a water bath for 30 minutes with frequent shaking. After allowing the mix to cool for 
a few minutes, pour it, with stirring, into a 500-mL beaker of cold water. Dinitrobenzene crystals 
should have formed. Filter the crystals to collect them, wash with water, press them with another 
piece of filter paper to squeeze out any excess liquid, and then recrystallize from ethyl alcohol. Yield 
is about 10-12 g. 



2,4-dinitrophenetole x a Y b z c 


1 


X 

z * 

unknown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: MSDS 


GhemAlcrl* 
Siorage Coda 

GRAY 




Synonyms: 


Synthesis: Nothing yet 



A 



B-(2,4-dinitrophenoxy) ethanol 


(0 2 N) 

2 c 6 h 3 och 2 ch 2 

(0N0 2 ) 


1 






mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 1SDS 


LAflGliARD* | 
Storage Code 


no 2 


Synonyms: dinitrophenylglycolether nitrate; glycoldinitrophenylether nitrate 


Synthesis: I know very little about this compound, it is an explosive, but the synthesis details are too 
sketchy for inclusion in its own page. 

It can be prepared from dichlorobenzene and ethylene glycol, followed by nitration of the resulting 
glycol monophenyl ether. 



http://www.roguesci.org/megalomania/synth/synthesis2.html (9 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 




dioxane 


c 4 h 8 o 2 


mp 11.80 


bp 101.1 


d 1.0329 


m 88.11 



Safety Data: ISPS 



1 

c $?.?? 




LA&GUAIRD* 
Stu-raga Coeb 



Jk 




Synonyms: diethylene dioxide; 1,4-diethylene dioxide; diethylene ether; diethylene oxide; 1,4- 
diethyleneoxide; diokan; Diox; 1,4-dioxacyclohexane; 1,4-dioxane; p-dioxane; dioxyethylene ether; 
ethylene glycol ethylene ether; glycol ethylene ether; tetrahydro- 1,4-dioxin; tetrahydro-p-dioxin 

Synthesis: Nothing yet 



ethyl acetate 


CH 3 COOC 2 H 5 


1 


mp -83 bp 77 d 0.898 


m 88.11 


; $?.?? 


Safety Data: 1SDS Flammable 


LABGUAFiD* ! 
StO’cicje Cobb 



Synonyms: acetic acid ethyl ester ; acetic ester; acetic ether; acetidin; acetoxy ethane; ethyl acetic 
ester; vinegar naphtha 



Synthesis: Prepare a mixture of 50 mL of ethyl alcohol and 50 mL of 98-100% sulfuric acid in a 

round-bottomed 500-mL Florence flask. Set the flask up for simple distillation with addition. Heat 
the mixture with an oil bath, when the temperature of the oil reaches 140 °C slowly add a mixture of 
400 mL of ethyl alcohol and 400 mL of glacial acetic acid through the addition funnel. Control the 
addition of the acid mix to correspond to the rate at which the product distills over. 

Once the reaction has been completed, transfer the distillate to a beaker. Treat the distillate with a 
dilute solution of sodium carbonate to neutralize any acetic acid that has passed over. Test the pH of 
the upper layer; it should be basic. Transfer the neutralized distillate to a separatory funnel, and drain 
off the lower layer. Filter the remaining layer to remove any contaminants, and then pour the 
solution back into the separatory funnel. 

Prepare a solution of 100 g of calcium chloride in 100 mL of water. Add this solution to the 
separatory funnel to remove any excess alcohol, shake the funnel well. The calcium chloride can 
also be added in portions if desired, drain off the lower each time. After shaking, dry the upper layer 
by transferring it to a small Erlenmeyer flask with a layer of granular calcium chloride in the bottom. 
Filter the dried product to remove the calcium chloride, transfer the filtrate to a Florence flask, and 
then simple distill to collect pure ethyl acetate. Yield can be as high as 90%. 



http://www.roguesci.org/megalomania/synth/synthesis2.html (10 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 





ethyl alcohol C 2 H 5 OH 


1 




mp 114.1 bp 78.5 d 0.789 m 46.07 


;$?.?? 


Safety Data: MSDS 


LABGUARD* I 
Stoj-ayu Coee 


Synonyms: ethanol ; absolute alcohol; alcohol; alcohol dehydrated; algrain; anhydrol; anhydrous 
alcohol; booze; cologne spirits; dehydrated alcohol; denatured alcohol; ethanol 200 proof; ethyl 
hydrate; ethyl hydroxide; fermentation alcohol; grain alcohol; hooch; jaysol; jaysol s; liqueur; 
methylcarbinol; molasses alcohol; moon shine; potato alcohol; sd alcohol 23-hydrogen; spirits; 
spirits of wine; Synasol; tecsol 


Synthesis: Nothing yet 





ethyl chloride C 2 H 5 C1 


1 




mp -138.7 bp 12.3 d 0.9214 m 64.51 


;$?.?? 


Safety Data: MSDS 


LABGUARD* I 
StCW-SOB CdEE 


Synonyms: chloroethane; aethylis; aethylis chloridum; Anodynon; Chelen; chlorene; chlorethyl; 
chloridum; chloryl; Chloryl Anesthetic; cloretilo; dublofix; ether chloratus; ether hydrochloric; ether 
muriatic; hydrochloric ether; Kelene; monochloroethane; muriatic ether; Narcotile 


Synthesis: Nothing yet 



ethylene dichloride C1CH 2 CH 2 C1 


1 


X 

W"7 ? x 
Z 1 
unknown 


mp -40 bp 83-84 d 1.2569 m 98.96 


; $?.?? 


Safety Data: Flammable, Toxic 


iabguard* 


Synonyms: 1 ,2-dichloroethane\ Brocide; sym-dichloroethane; Dutch liquid; EDC; ethylene chloride 


Synthesis: Nothing yet 



http://www.roguesci.org/megalomania/synth/synthesis2.html (11 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 





ethylene glycol HOCH 2 CH 2 OH 


1 


.. . OH 

HUT 


mp -13 bp 197.6 d 1.1135 m 62.07 


c $?.?? 


Safety Data: MSDS 


jLABGUARD* 

: Storage Code 

GREEN 


Synonyms: 1,2-ethanediob, 1,2-dihydroxyethane; Dowtherm 4000; Dowtherm SR 1; EG; ethane-1, 2- 
diol; ethylene alcohol; ethylene dihydrate; Fridex; glycol; glycol alcohol; lutrol-9; macrogol 400 
bpc; M.E.G.; monoethylene glycol; norkool; tescol; ucar 17 


Synthesis: Nothing yet 



ethyl ether C 2 H 5 OC 2 H 5 


1 




mp -116.3 bp 34.6 d 0.7134 m 74.12 


;$?.?? 


Safety Data: Flammable 


LABGUARD* | 


Synonyms: l,F-oxybisethane\ anesthetic ether; diethyl oxide; diethyl ether; ether; ethoxyethane; 
ethyl oxide; pronarcol; sulfuric ether 



Ether is a very useful organic solvent that has fallen into ill repute because of its use by drug dealers. 
It is a watched chemical by the DEA, purchasing large quantities will put you on The List. Ether is 
an explosively flammable liquid that will easily fill a room with fumes just waiting to be ignited by 
the slightest heat, it ignites over 180 °C. Keep containers of ether tightly closed and away from all 
flame sources. Ether used to be an anesthetic back in the days, inhaling the fumes will cause 
unconsciousness, but not much damage if you get to fresh air. Ether can also form an explosive 
peroxide if it is old or exposed to air. In short, keep ether away from all flame, in a well ventilated 
area, and tightly sealed in its container. You might think that ether and water do not mix, wrong, 
ether can hold up to 1.2% water. The only OTC source of ether is in starting fluid for cars, among 
other contaminants, from which it can be distilled. Ether can easily be prepared by reacting ethyl 
alcohol with sulfuric acid. 

Synthesis: Assemble the necessary equipment for fractional distillation, adding in a Clasien adapter. 
Place the fractionating column on the side arm of the Clasien, and a 2-holed rubber stopper in the 
straight arm. In the first hole, place a thermometer that extends to near the bottom of the reaction 
flask. In the second hole, place a length of glass tubing that extends to near the bottom and sticks up 



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Megalomania's Precursor Section Part 2 



about an inch. Place a short length of rubber tubing on the glass tubing and connect it to an addition 
funnel. The rubber tubing is to slightly offset the funnel which would get in the way of the 
thermometer. If using a 500-mL reaction flask, add 146 mL of anhydrous ethyl alcohol. You can use 
95% alcohol but the efficiency of the reaction will suffer because of the water. Slowly add 133 mL 
of anhydrous sulfuric acid, again you can use less than 100%, but the more water there is the worse 
the reaction will proceed. Place a magnetic spin bar in the flask and connect it to the rest of the 
apparatus. Using a hotplate or oil bath, no flame, heat the reaction flask, while stirring, to between 
130-140 °C and hold it at that temperature. Be sure not to go in excess of 150 °C as ethylene gas will 
be produced. Once some distillate starts to come over, slowly add an additional 146 mL of ethyl 
alcohol from the addition funnel at the same rate as is collected from the distillation. That should be 
about a drop or two a second. The total distillation time should be over 2 hours. After the distillation 
is over, pour the distillate from the receiver flask to a large beaker and add 10% sodium hydroxide 
solution until the pH is neutral. Pour this mixture into a seperatory funnel and allow the lighter ether 
layer to float on top. Remove the heavier water layer and wash the remaining ether by shaking twice 
with a volume of saturated salt water equal to the volume of ether. Allow the last wash to sit for 
several minutes to insure complete seperation then remove the water layer. Put the ether in a 
Florence flask and add 15 g of calcium chloride for every 100 mL of ether, stir this for 2 hours with 
a magnetic stirrer. Finally, do a simple distillation to remove the now anhydrous ether from the 
calcium chloride. 



formaldehyde 


HCHO 


mp -92 


bp -19.5 


d 1.067 


m 30.03 



Safety Data: Flammable, Toxic 



Synonyms: BFV; fannoform; formaldehyde solution; Formalin; Formalin 40; formalith; formic 
aldehyde; Formol; FYDE; HCHO; HOCH; karsan; lysoform; Methan 21; methanal; methyl 
aldehyde; methylene glycol; methylene oxide; Morbicid; oxomethane; oxomethylene; 
oxymethylene; superlysoform; Veracur 




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Megalomania's Precursor Section Part 2 



Synthesis: Formaldehyde can be obtained at Wal-Mart stores in a variety of products called 

Campa Chem for use in recreational vehicle sewage treatment (in the automotive section). There is 
one brand that is solid granules, get that, not the solution. The actual chemical is paraformaldehyde, 
the polymerized form of formaldehyde, but formaldehyde can be obtained from this. 

Campa Chem paraformaldehyde is dyed blue for some reason with an unknown chemical. As this 
may or may not affect some chemical reactions it is best to remove it. One of the simplest ways is to 
extract the dye with numerous small portions of alcohol. Empty the packets (a box comes with ten 2 
oz packets) in a beaker and add 40 mL of ethyl or methyl alcohol per packet to wet the powder. Two 
packets for example will require about 1 L of ethyl alcohol to extract most of the blue dye. You 
should add only 20-25 mL at a time, stir, and pour off the alcohol. 

You may lose a little of the paraformaldehyde when you decant off the alcohol, so a filter may 
help. With each successive extraction more of the dye will be removed. The dark blue alcohol 
extract can be simple distilled to recover pure alcohol. The resulting paraformaldehyde granules may 
still have a slight blue tint, but significant quantities of the dye will be gone. 

To obtain a formaldehyde solution add 100 g of paraformaldehyde granules to a bottle and dilute 
with enough water to make 250 mL of solution. Add a small amount of sodium hydroxide, 
approximately 120 mg, to the solution. Cap the bottle and shake to dissolve some of the 
paraformaldehyde. Place the bottle into a hot water bath heated to 60 degrees C for 25-30 minutes. 
Every 5 minutes shake the bottle and open it to vent any gasses. Some of the paraformaldehyde may 
not have dissolved, it can be filtered off, or heat the bottle longer. The resulting formaldehyde 
solution should be about 40% and will remain fresh for a few days if refrigerated. 

Not everyone may be able to get to Wal-Mart, so here is a synthesis of formaldehyde from scratch: 

The side tube (length about 10 cm) of a distilling flask (capacity 250-mL) is bent upwards at the 
junction with the neck of the flask. The end of the side tube, drawn out into a capillary (internal 
diameter 1.0- 1.5 mm), is then inserted through a cork into a piece of combustion tubing about 30 cm 
long (fig 53). Within the tubing and about 6 cm from the point of the capillary is a copper spiral 4 
cm long. The tubing slopes upwards at a small angle and its upper end is connected with a vertical 
condenser, preferably of the coil type. To the lower end of the condenser there are attached two 
communicating receivers which, during the experiment, are almost completely immersed in a 
freezing mixture. The short side tube of the second receiver is connected to an air pump (like a fish 
tank pump). Into the distilling flask, which is lowered as deeply as possible into a water bath kept 
exactly at 46-47 degrees C, 100 mL of methyl alcohol are poured. The flask is then closed with a 
rubber stopper, through which is inserted a glass tube reaching nearly to the bottom. Through this 
tube air is drawn in, and when the air is passing, the copper spiral is warmed in the flame, cautiously 
at first, until, when red heat is reached, the reaction sets in. 

The air current must now be so regulated that the spiral continues to glow quite feebly without 
further application of heat. If the experiment is carried out in this way there will be complete 
freedom from explosions. The region within which methyl alcohol-air mixtures explode is indeed 
reached when the temperature of the bath is too low (42-44 degrees C), but the flame strikes back no 
further than the capillary tube, since the rapid current in the latter prevents further striking back. This 
is why it is very important to keep the water bath at 46-47 degrees C. 

The two receivers contain 110-115 mL of a 30-32% formaldehyde solution after all the methyl 



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Megalomania's Precursor Section Part 2 



alcohol has been evaporated. A further small quantity of formaldehyde may still be collected in a 
third receiver containing a little water. 

The following paragraph contains some points which should be considered in carrying out gaseous 
reactions. 

In order to dehydrogenate one mole of methyl alcohol 0.5 mole of oxygen is required, and hence 
for one volume of the alcohol half as much oxygen or two and a half times as much air. The 
stoicheiometrical must therefore contain methyl alcohol and air in the proportions (by volume) 1 : 
2.5, ie. 28.5% of methyl alcohol. Since the volumes vary as the partial pressures the temp of 
evaporation (of the alcohol) must be so chosen that its vapor pressure shall be 28.5% of the 
atmospheric pressure, ie. About 210 mm of mercury. With the simple type of apparatus here 
described complete saturation of the air with methyl alcohol vapor is not reached, and hence a 
temperature somewhat higher than the theoretical is used. 




formamide 


hconh 2 


1 


mp 2.55 


bp 210.5 


d 1.13340 


m 45.04 


c$?.?? 




http://www.roguesci.org/megalomania/synth/synthesis2.html (15 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 



Safety Data: SDS 


jLABGUARD* 

:i Siofags Code 




GREEN 











Synonyms: carbamaldehyde; formimidic acid; methanamide 



Synthesis: Nothing yet 



formic acid 


HCOOH 


1 


0 


mp 8.4 bp 100.8 d 1.220 


m 46.03 


c $?.?? 


Safety Data: Corrosive 


LABGUARD* 
Storage Code 

WHITE 




Synonyms: ameisensaure; aminic acid; formylic acid; hydrogencarboxylic acid; methanoic acid 


Synthesis: Nothing yet 



gasoline mixture 


1 


No 

Graphic 


mp? bp 32-210 d? m- 


: $?.?? 


Safety Data: Flammable 


LABGUARD* I 
StO^-SuB Code 


Synonyms: Benzin; gas; gasahol; gasolene; light gasoline; motor fuel; motor spirits; natural 
gasoline; petrol; premium; super; unleaded 


Synthesis: Coming soon! 



glycerol 


CH 2 OHCHOHCH 2 OH 


1 


mp 17.8 


bp 290 (dec) 


d 1.26362 


m 92.09 


c $?.??^ 





Safety Data: MSDS 



| LABGUAHD*" 
: Sloiacje Cuds 

GREEN 




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Megalomania's Precursor Section Part 2 





Synonyms: 1,2,3-propanetriol; Bulbold; Cristal; Glyceol; glycerin; glycerine; glycerin mist; 
glyceritol; D-glycerol; L-glycerol; glycyl alcohol; IFP; incorporation factor; Ophthalgan; polyhydric 
alcohols; propanetriol; trihydroxy propane; 1,2,3-trihydroxypropane 




Synthesis: Coming soon! 



HBIW 


X a Y b Z c 


1 


X 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: MSDS 




ChemAlcrl* 
i Storage Code 






GRAY 


Synonyms: 



Synthesis: Nothing yet 



n-hexane 


CH 3 (CH 2 ) 

4 CH 3 


1 


X 

W"/ ? x 

z 1 

unknown 


mp-100 bp 69 d 0.660 


m 86.18 


; $?.?? 


Safety Data: Flammable 


LABGUARD* ! 
Code 


Synonyms: dipropyl; gettysolve-b; Hex; hexane; hexyl hydride; normal hexane; skellysolve B 


Synthesis: Nothing yet 



hydrazine 


h 2 nnh 2 


1 


h 2 h nh 2 


mp 2 bp 113.5 d 1.0036 


m 32.05 


: $?.?? 


Safety Data: Corrosive, Toxic 


LAtiGiUAfiD* | 
Code 



Synonyms: anhydrous hydrazine; diamide; diamine; hydrazine base; hydrazine, hydrazine sulfate 



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Megalomania's Precursor Section Part 2 



Synthesis: Prepare a solution of 1500 mL of 28-29% ammonium hydroxide, 900 mL of water, 375 

mL of 10% gelatin solution, and 1200 mL of normal sodium hypochlorite solution. It is absolutely 
imperative to use distilled water, the presence of any contaminant ions will screw up this reaction! It 
is possible to use starch, glue, or glycerol instead of gelatin, but they are inferior. Mix these 
chemicals in a large glass dish, like a pie plate or bowl, or just use several portions, as this is nearly a 
gallon of liquid. This mixture is heated as rapidly as possible and boiled down to one-third of its 
original volume. The solution is then cooled thoroughly with ice and suction filtered twice to remove 
any impurities. When filtering, first use towels (like a washcloth), then use regular filter paper on top 
of some cloth (like from a T-shirt). 

The resulting liquid is dilute hydrazine hydrate. To make concentrated hydrazine hydrate, mix 
144 mL of dilute hydrazine with 230 mL of xylene in a round-bottomed 500-mL Florence flask. 
Fractionally distill the mixture in an atmosphere of nitrogen, the xylene will first pass over with 
most of the water, then the hydrazine will pass over. Keep the fractions separate of course. The 
resulting hydrazine hydrate will be 90-95% hydrazine. This concentration procedure is meant for 
60% hydrazine hydrate, since the hydrazine hydrate prepared above may be greater or less than 60%, 
some experimentation may be needed to find the proper amount of xylene to use (more xylene is 
needed for dilute hydrazine, less for more concentrated hydrazine). 

To obtain anhydrous hydrazine, mix 20 g of potassium hydroxide per 100 g of >90% hydrazine 
hydrate in a beaker, let this mixture stand overnight so much of the water can be withdrawn. After 
standing, filter the solution to remove the hydroxide. Add to the filtered liquid an equal amount by 
weight of sodium hydroxide. Place this mixture in a round-bottomed 500-mL Florence flask, reflux 
for 2 hours, then distill in a slow stream of nitrogen. You must use nitrogen, distillation in air may 
lead to an explosion! 



hydrochloric acid 


HC1 


1 


H Cl 


mp -46.2 bp 108.58 d 1.15 


m - 


c $?.?? 


Safety Data: Corrosive 


LABGUARD* 
Storage Coda 

WHITE 





Synonyms: chlorohydric acid; hydrochloride; hydrogen chloride; muriatic acid; spirits of salts 



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Megalomania's Precursor Section Part 2 



Hydrochloric acid is actually a mixture of hydrogen chloride gas in water, not a single compound. 
The physical data provided here is for 30% hydrochloric acid, the most common varity. The 
maximum concentration of acid is about 40%. 

Synthesis: Adding concentrated sulfuric acid to large chunks of ammonium chloride can generate 

hydrochloric acid (actually hydrogen chloride gas). The sulfuric acid is slowly added to the 
ammonium chloride kept inside a bottle. The bottle is sealed with a 2-holed stopper, in one hole goes 
an addition funnel where the sulfuric acid is added, and in the other goes a short length of glass tube 
bent at a right angle. The angled tube is the outlet tube for the hydrochloric acid, it can be connected 
to whatever experiment is needed, or bubbled into water to collect the acid for later use. Be careful 
not to allow acid gas to escape through the addition funnel, either use a stopcock, or keep the stem 
below the surface of the liquid. 

If anhydrous hydrogen chloride gas is required, using a similar glassware setup as above, add 
hydrochloric acid very slowly through the addition funnel into concentrated sulfuric acid. The 
hydrochloric acid gas that evolves is dried by bubbling it through a safety wash bottle filled with 
concentrated sulfuric acid. To set up a safety wash bottle, affix a 2-hole stopper to a top of a bottle, 
in one hole goes a short length of glass tube bent at a right angle; this is the outlet tube. In the other 
hole, place a wide diameter glass tube that extends just below the surface of the sulfuric acid. Place a 
second small diameter glass tube inside the wide tube. This tube should nearly reach the bottom of 
the bottle, it should also be bent at a right angle at the top to keep it from falling in. This is the inlet 
tube for the acid to be washed. See the illustration. This setup is necessary to prevent the acid wash 
from being sucked back into the generator. 

Hydrochloric acid can also be generated by heating 10 parts of sodium chloride with a cold 
mixture of 3 parts of water and 18 parts of sulfuric acid. 



hydrogen 


h 2 


1 


X 

Wv 

z x 

uhknown 


mp -259.2 


bp 252.77 


d 0.0700 


m 2.0158 


2 $?.?? 


Safety Data: MSDS 


LASGUARD* ! 
Cdce 


Synonyms: protium 


Synthesis: Coming soon! 




hydrogen peroxide 


h 2 o 2 


1 


H --.| 

cr h 


mp -0.43 


bp 152 


d 1.463 


m 34.01 


2 $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis2.html (19 of 20)12-8-2004 17:24:16 



Megalomania's Precursor Section Part 2 





Safety Data: MSI Corrosive 


C hem Alert 1 
Storage Code 

YELLOW 






Synonyms: Albone; dihydrogen dioxide; high-strength hydrogen peroxide; Hioxy; H202; hydrogen 
dioxide; hydroperoxide; Inhibine; Lensan A; Mirasept; Oxydol; Oxysept; Pegasyl; Perhydrol; 
Peroxan; peroxide; superoxol; t- stuff 


Synthesis: Coming soon! 





A 



hydroquinone x a Y b z c 


1 


X 

W'"/ ? X 

z 1 

utiknovm 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl 1 
Sic rage Coda 

GRAY 




Synonyms: 


Synthesis: Nothing yet 



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Megalomania's Controversial Chem Lab ©1997-2004 /synthesis2/ revised March 10, 2004 



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Cost 



This page is not done yet. 



http://www.roguesci.org/megalomania/synth/cost.htmll2-8-2004 17:24:16 




Megalomania's Precursor Section Part 4 



Precursors Part 4 



A 



2-nitro- 2- (m-nitropheny 1) - 
propanediol- 1,3 


X a Y b Z c 


1 


X 

W"7 ? n 
z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl* 
i Sic rage Coda 

GflAV 

1— *— ■■■ — 




Synonyms: 


Synthesis: Nothing yet 



1 -nitropropane CH 3 CH 2 CH 2 NO 2 


1 


X 

W"/ ? \ 

z 1 

unknown 


mp -108 bp 131.6 d 0.9934 m 89.09 


c $?.?? 


Safety Data: 1SDS 


ChemAlcrl* 

; Siorage Coda 




Synonyms: 


Synthesis: Nothing yet 



A 




2-nitropropane 


CH 3 CH 

(N0 2 )CH 3 


1 


X 

W"/ ? x 

z 1 

unknown 


mp -93 bp 120.3 d 0.9821 


m 89.09 


c $?.?? 


Safety Data: 


ChemAlcrl * 
i Siorage Coda 

GRAY 





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Megalomania's Precursor Section Part 4 



Synonyms: 



Synthesis: Nothing yet 




A 



nitrosyl tetrafluoroborate NOBF 4 


1 


X 

W"7 ? n,, 

z x 

unknown 


mp? bp? d 2.185 m 116.81 


c $?.?? 


Safety Data: 


ChemAlcn 4 
i Storage Coda 

GflAV 

— 




Synonyms: nitrosonium tetrafluorborate; nitrosyl fluoborate; nitrosyl fluoride 


Synthesis: Nothing yet 



A 



A 



nitrous oxide N 2 0 


1 


Nw 

L N 


mp -90.81 bp -88.46 d- m 44.01 


2 $?.?? 


Safety Data: 


! LABGUAHD* 

: Storage Code 






GREEN 


Synonyms: dinitrogen monoxide; dinitrogen oxide; factitious air; hyponitrous acid anhydride; 
laughing gas; nitrogen oxide 


Synthesis: This is listed as a potential undesired byproduct of explosive manufacture, but its drug 
properties make it a good candidate for inclusion in The Pharmacy. 







oxalic acid 


X a Y b Z c 


1 


X 

W"7 ? n 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


Chem Alert* 
Storage Code 

• . .. 





Synonyms: 



http://www.roguesci.org/megalomania/synth/synthesis4.html (2 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 



Synthesis: Oxalic acid is available OTC in hardware stores as a generic cleaning agent. It is sold 

as a reasonably pure powder in approximately 500 g boxes depending on brand. 

It is often desirable to use anhydrous oxalic acid; it can be dried by the following procedure. 
Place a glass casserole dish or pie plate in an oven and preheat it to 100 °C. When the temperature 
has been reached, remove the dish and rapidly cover it with a uniform layer of finely pulverized 
oxalic acid, quickly return the dish to the oven. The layer of acid should not be more 3-4 mm thick, 
and should be as finely powdered as possible to insure maximum dehydration. Let the acid cook for 
2 hours. 

When finished, the product is removed, crushed if slightly caked, and quickly bottled to keep it 
away from moisture. The exact quantity that can be dried is dependant on the size and number of 
plates you use. A certain portion of oxalic acid will sublime during heating, and this portion may 
eventually be harmful to the metal of the oven. I suggest you crank up the heat for another hour 
when done to drive off any remaining vapors, then give the oven a washing to prevent any 
contamination, even if this oven is not used to cook food with. 



oxanilide 


C 14 H 12 N 2°2 


1 


o 

o 

- ; y z 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


Chem Alert* 

. Siarage Coda 

GflAV 




Synonyms: N,N'-diphenyl-ethanediamide; oxaldianilide 


Synthesis: This substance has been used as an antiflash agent in propellants, and as a coolent and 

burning rate reducer in fuzes. To synthesize, mix two parts of oxalic acid with one part of aniline in 
a round bottom flask. Stir and heat the mixture until the reaction is complete as evidenced by the 
cessation of effervescence. The mass should be cooled to room temperature, poured into several 
volumes of water cooled to 21-24 °C, then filtered on a Buchner funnel. The material on the funnel 
is washed free of oxalic acid with water, and then washed free of aniline with acetone. The washed 
material is dried at 100-110 °C. 









oxygen 


0 2 


1 




mp -218.4 


bp -182.96 


d- 


m 32 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis4.html (3 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 





Safety Data: 




LAftGUAnD* ! 
Storage Col; e 


X 

W"/ ? v 

z 1 

unknown 


Synonyms: GOX; LOX 


Synthesis: Coming soon! 



paraffin 


mixture of 

C n H 2n + 2 


1 


X 

W"/ ? N 

z 1 

unknown 


mp 50-57 bp ? d 0.90 


m - 


c $?.?? 


Safety Data: 


jLABGUARD* 

: Storage Coda 

GREEN 




Synonyms: hard paraffin; paraffin wax 


Synthesis: Nothing yet 



paraformaldehyde (CH 2 0) n 


1 


X 

W"/ ? N 

z 1 

unknown 


mp - bp - d ? m - 


; $?.?? 


Safety Data: Corrosive, Flammable 


LAflGUARD* | 


Synonyms: Formagene; Paraform; poly oxy methylene; triformol; trioxymethylene 


Synthesis: Nothing yet 



paraldehyde 


C 6 H 12°3 


1 


mp 12 


bp 124 


d 0.994 


m 132.16 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis4.html (4 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 





Safety Data: 


ChemAlcrl* 

; Siorage Code 

GflAV 




X 

W"/> 

z 1 

unknown 


Synonyms: 2,4,6-trimethyl-l,3,5-trioxane\ paracetaldehyde; Paral 


Synthesis: See the end of acetylaldehyde for the Synthesis of paraldehyde. 





A 



Pearlman's catalyst X a Y b Z c 


1 


X 

W"/ ? y 
z 1 

unknown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: 1SDS 


ChemAlcrl* 
Storage Code 

- — _ 




Synonyms: 


Synthesis: Nothing yet 



A 



pentaerythritol 


C 5 Hi 2 0 4 


1 


HO 

HO 


mp 260 


bp ? 


d? 


m 136.15 


c $?.?? 


Safety Data: 


ChemAlcrl* 
Siorage Code 

GflAf 









Synonyms: 2,2-bis(hydroxymethyl)-l,3-propanediol; Hercules P 6; monopentaerythritol; PE 200; 
pentaertyhrito; PETP; tetrakis(hydroxymethyl)methane; tetramethylolmethane; THME 



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Megalomania's Precursor Section Part 4 



Synthesis: Prepare a solution of 800 g of paraformaldehyde and 165.5 mL of acetaldehyde in 5.5 

L of water. Add to this solution 180 g of powdered calcium oxide in small portions with rapid 
stirring, a mechanical stirrer is advised. The rate of addition of the calcium oxide is adjusted such 
that the temperature of the solution rises to 50 °C over a 30 minute period with the first portion. The 
addition of each subsequent portion should not be allowed to raise the temperature above 55 °C. 
After the addition is complete, stirring is continued for 3 hours. The solution will become yellowish. 
After stirring, the solution is filtered to remove any contaminant particles, and the yellow filtrate is 
acidified with just enough hydrochloric acid to make it acid to litmus paper. It is recommended to 
decolorize the filtrate; add the decolorizer, stir for 5 minutes, and then filter again. 

The colorless filtrate is now concentrated under reduced pressure until crystals begin to separate. 
Since it is rather inconvenient to run the entire lot, divide the solution into portions. The 
concentration can be done with a vacuum distillation setup. Using a 500-mL flask, add 200-300 mL 
of solution, when 40% of the water (80-120 mL) has boiled over, stop the distillation and add the 
next portion. Eventually you should have approximately 3 L of concentrated solution left. Heat this 
solution on a steam bath, while hot, suction filter it to remove any contamination. Any precipitated 
crystals that get caught on the filter can be washed through by wetting with steam. The filtrate is 
now allowed to stand in a refrigerator overnight, whereupon the first crop of crystals will 
precipitate. These crystals are filtered to collect them. The filtrate is then boiled down to about 2 L, 
and again refrigerated overnight. A second crop of crystals will form; these can be filtered to collect 
them like before. The filtrate is now boiled down to about 1 .2 L, refrigerated overnight, and the 
subsequent crystals are collected by filtration. The filtrate is finally boiled down to the consistency 
of syrup, refrigerated overnight, and the last crop of crystals is collected by filtration. 

The combined crystals, which should weigh as much as 410-420 g, are recrystallized from an 
equal weight of hot water containing 10 mL of concentrated hydrochloric acid. This new solution 
can be decolorized, and then boiled down to obtain several additional crops of pure crystals. Discard 
the last 30-40 mL. The yield is about 55-57%. 



perchloric acid HC10 4 


1 


X 

Z x 
unlmown 


mp-112 bp dec d 1.768 m 100.46 


c $?.?? 


Safety Data: Corrosive, Oxidizer 


LABGUARD* 
Storage Code 

WHITE 










Synonyms: 


Synthesis: Coming soon! 



http://www.roguesci.org/megalomania/synth/synthesis4.html (6 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 






perchloryl fluoride C1F0 3 


1 


X 

z x 

unknown 


mp -147.7 bp -46.7 d- m 102.45 


c $?.?? 


Safety Data: 


ChemAlcrl* 
Siorage Code 

GRAY 




Synonyms: 


Synthesis: Nothing yet 



a 







petroleum ether mixture 


1 


X 

^"/ ? > 
z 1 

unknown 


mp - bp 90-155 d 0.860 m- 


; $?.?? 


Safety Data: Flammable 


LAflGUAfiD* 


Synonyms: benzin; Benzoline; Canadol; ligroin; ligroine; naphtha petroleum; naphtha, VM&P; 
petroleum naphtha; petroleum spirits; refined solvent naphtha; solvent naphtha; varnish makers' & 
painters' naphtha; V.M.&P. naphtha 


Synthesis: Petroleum ether, or ligroin, is a very common solvent made up of a mixture of all the 

crap left over from petroleum industries. As such, it can't really be synthesized without extensive 
resources and equipment, it is far easier just to buy it. Petroleum ether is not all that expensive or 
hard to get, it is available OTC in hardware and paint stores as a paint solvent, usually under the 
name of VM&P naphtha. It retails around $2.70 a liter. VM&P naphta stands for Varnish Makers 
and Painters naphtha. 


_ 





phenol 


C 6 H 5 OH 


1 




mp 43 bp 182 d 1.071 


m 94.11 


c $?.?? 


Safety Data: Corrosive, Toxic 


LABGUARD* 
Storage Code 

WHITE 





Synonyms: baker's p and s; benzenol; carbolic acid; hydroxy benzene; monohydroxy benzene; 
monophenol; oxy benzene; phenic; phenic acid; phenol alcohol; phenyl hydrate; phenyl hydroxide; 
phenylic acid; phenylic acid, phenyl hydroxide; phenylic alcohol 



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Megalomania's Precursor Section Part 4 



Synthesis: Pour 18.2 mL of 95-100% sulfuric acid as rapidly as possible, with stirring, into 50 mL 

of water in a 500-mL beaker. Add to the hot solution 10 g of freshly distilled aniline, with stirring, 
by allowing it to flow down the side of the beaker. Next add 100 mL of water. Place the beaker into 
a cold water bath so it may cool to room temperature, it is then treated with a solution of 8.5 g of 
sodium nitrite in 40 mL of water, until it shows a blue spot on starch-potassium-iodide paper. If you 
do not have the paper, add it all. The beaker will now contain diazobenzene sulfate, this is gently 
heated to 40-50 °C for 30 minutes to convert it to phenol. 

The phenol that should have formed is removed by steam distillation. Add a large enough 
quantity of salt to the distillate so it becomes saturated, the solution is now extracted several times 
with ether. Add a small amount of sodium sulfate to the combined ether extracts and let it stand for 
a few hours. The ether is then evaporated, and the residue of phenol is simple distilled. The yield is 
about 7-8 g. 

The liquid that remains in the flask after the steam distillation contains oxydiphenyl. It can be 
disposed of, or filtered hot. Upon cooling crystals will form. 



phosphorus X a Y b Z c 


1 


X 

z 1 

unknown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl* 
Sic ra ge Code 




Synonyms: 


Synthesis: Nothing yet 



phosphorus oxychloride POCl 3 


1 


X 

W"/ ? N 

z 1 

unknown 


mp 1.25 bp 105.8 d 1.645 m 153.33 


c $?.?? 


Safety Data: Corrosive 


LABGUARD* 
Storage Code 

WHITE 




Synonyms: phosphoryl chloride ; phosphorus chloride 


Synthesis: Coming soon! 



http://www.roguesci.org/megalomania/synth/synthesis4.html (8 of 16)12-8-2004 17:24:19 




Megalomania's Precursor Section Part 4 






phosphorous pentoxide P 2 O 5 


1 


X 

z 1 

unknown 


mp 340 bp 360 d2.30 m 141.94 


c $?.?? 


Safety Data: Corrosive 


LABGUARD* 
Storage Code 

WHITE 




Synonyms: diphosphorus pentoxide; phosphoric anhydride 



Synthesis: Nothing yet 



phosphorus trichloride 


PC1 3 


1 


X 

W"/ ? X 

z 1 

unknown 


mp -112 bp 76 d 1.574 


m 137.33 


c $?.?? 


Safety Data: MSDS 


GhemAierr 
Siarage Coda 

Gfl/W 







Synonyms: phosphorous chloride 



Synthesis: Under water, in a shallow dish, cut 40 g of white phosphorus into small pieces with a 

knife. Displace the air in a 250-mL Florence flask with dry carbon dioxide. Add each piece of 
phosphorus to the flask by removing it from the water with tweezers, drying quickly by pressing 
between several layers of paper towel, and immediately placing in the flask. Be extremely careful 
that you do not ignite the phosphorus by friction from the paper towel, or by dropping it against the 
next of the flask. As soon as all of the phosphorus has been added, set the flask up for simple 
distillation with addition. Instead of a separatory funnel on the Clasien adapter, seal the straight arm 
with a 1-hole stopper or a thermometer adapter. Into the hole place a straight length of glass tubing 
far enough into the flask such that it is just above the level of the phosphorus. Do not run water 
through the condenser. The receiving flask should be held under a shower of cold water, and in a 
cold water bath, for example under a running faucet, and in a bowl that can overflow into the sink. 
There will be substantial quantities of waste chlorine gas, if you are using a vacuum adapter to 
connect the condenser to the receiver, attach a hose to it so it may direct the gas elsewhere. If not, 
you will figure something out, or you will suffocate. 

A moderately rapid current of dry chlorine gas is passed over the white phosphorus; phosphorus 
trichloride will form with the evolution of heat and light. Some crystals of phosphorus pentachloride 
may begin to clog the condenser, these can be dislodged by gently heating the condenser, or by 
increasing the flow of the chlorine to generate more heat. If some white phosphorus begins to distill 
over, reduce the flow of the chlorine, or try to cool the reaction flask by briefly immersing it in cold 
water. The phosphorus trichloride thus collected is purified by distillation. 



http://www.roguesci.org/megalomania/synth/synthesis4.html (9 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 



picramic acid 


c 6 h 5 n 3 o 5 


1 


\ 

H + p 


mp 169 bp - d ? 


m 199.12 


c $?.?? 


0 / 




H > 

/ \ 

HO HH 2 


Safety Data: 


LABGtJARD* | 
StQr.ayB Coda) 







Synonyms: 2-amino-4,6-dinitrophenol; 6-amino-2,4-dinitrophenol; dinitroaminophenol; 2,4-dinitro- 
6-aminophenol; 4,6-dinitro-2-aminophenol; 2-hydroxy-3,5-dinitroaniline; picraminic acid 




Synthesis: Nothing yet 









picryl chloride C 6 H 2 C1N 3 0 6 


1 


X 

W"/ ? N 

z - 1 

unknown 


mp 83 bp? d 1.797 m 247.55 


c $?.?? 


Safety Data: 4SDS 


ChemAierr 
Sic rage Code 

GRAY 




Synonyms : 2-chloro- 1,3,5- trinitrobenzene 


Synthesis: Nothing yet 



piperidine C 5 H U N 


1 


X 

W"/ ? v 

z 1 

unknown 


mp -7 bp 106 d 0.8622 m 85.15 


; $?.?? 


Safety Data: Corrosive, Flammable, Toxic 


LA&GUAflD* | 
Coae 


Synonyms: hexahydropyridine 


Synthesis: Nothing yet 



http://www.roguesci.org/megalomania/synth/synthesis4.html (10 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 



polystyrene ( c 8 H s)n 


1 


X 

z 1 

unknown 


mp - bp- d 1.04-1.065 m- 


c $?.?? 


Safety Data: 


ChemAlcrl* 
Siorage Code 

GflAV 




Synonyms: Dylene; styrofoam; Trycite 


Synthesis: Nothing yet 



A 



polyvinyl alcohol 


(CH 2 CHOH) 

n 


1 


X 

W|/S 
z 1 

unknown 


mp - bp - d ? 


m - 


c $?.?? 


Safety Data: 




ChemAlcrl* 
i Sierage Code 






GflAY 


Synonyms: ethenol homopolymer, Akwa Tears; Elvanol; Gelvatol; Liquifilm; Mowiol; Polyviol; 
PVA; Sno Tears; Vinarol; Vinol 


Synthesis: Nothing yet 



potassium carbonate K 2 C0 3 


1 


X 

W"/ ? N 

z 1 

unknown 


mp 891 bp? d 2.29 m 138.21 


c $?.?? 




Safety Data: 


jLABGUAHD* 

: Siorage Code 

GREEN 




Synonyms: pearl ash; salt of tartar 


Synthesis: Coming soon! 







potassium dinitroethanol 


X a Y b Z c 


1 





http://www.roguesci.org/megalomania/synth/synthesis4.html (11 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 




potassium hydroxide KOH 


1 


X 

W"/ ? -n 

z 1 

unknown 


mp 360 bp? d? m 56.11 


c $?.?? 


Safety Data: Corrosive 


LABGUARD* 
Storage Code 

WHITE 




Synonyms: caustic potash; potassa; potassium hydrate 


Synthesis: Coming soon! 



A 



potassium hypophosphite KH 2 P0 2 


1 


X 

#"/ ? JL 

z 1 

unknown 


mp dec bp - d ? m 104.09 


c $?.?? 


Safety Data: 


ChemAlcrO 
i Sis rage Code 

GflAY 




Synonyms: 


Synthesis: Nothing yet 



potassium iodide 


KI 


1 


mp 680 


bp- 


d 3.12 


m 166.00 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis4.html (12 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 





Safety Data: 


jjLABGUARD* 

| Siorage Code 

GREEN 




X 

z 1 

unknown 


Synonyms: Jodid; Thyroblock; Thyrojod 


Synthesis: Coming soon! 






potassium nitrate KN0 3 


1 


i 

o 

O 1 / tj 

\ 

p 


mp 333 bp 400 dec d 2.11 m 101.10 


c $?.?? 


Safety Data: Oxidizer 


C hem Alert 1 
Storaga Code 

YELLOW 







Synonyms: niter; nitric acid, potassium salt; saltpeter 


Synthesis: Coming soon! 





n-propyl alcohol CH 3 CH 2 CH 2 OH 


1 


X 

f'¥< y 

z 1 

unknown 


mp -127 bp 97.2 d 0.8016 m 60.10 


; $?.?? 


Safety Data: Flammable 


LABGUAiRD* | 


Synonyms: 1 -propanol, Optal; propylic alcohol 


Synthesis: Nothing yet 



propylene glycol 


CH 3 CHOHCH 2 OH 


1 




mp -59 


bp 188.2 


d 1.036 


m 76.10 


c$?.?? 


OH 




http://www.roguesci.org/megalomania/synth/synthesis4.html (13 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 



Safety Data: 



] LftBGUAHb* " 
: Storage Glide 

GREEN’ " 



Synonyms: 1,2-propanediol; 1,2-dihydroxypropane; methyl glycol 



Synthesis: This chemical can be found as a component in certain antifreeze as a non-toxic 

replacement for ethylene glycol. This Synthesis is for the laevorotatory version only, kind of like 
only left handed molecules versus a mixture of both left and right handed. This will not affect its 
usefulness. This Synthesis is kind of like fermenting alcohol. 

Prepare a solution of 1 Kg of sucrose in 9 L of water placed in a 20 L (5 gallon) bucket. Make a 
paste of baker's yeast by breaking up 1 Kg of yeast and gradually stirring in 1 L of water. This is 
then added to the sugar solution. Unless you have a way of sealing up the bucket, or you have a big 
bottle like a water cooler, I recommend pouring this solution into several 2-L plastic soda bottles, or 
gallon milk jugs. Cap each of the bottles with a one-hole rubber stopper and connect a length of 
rubber or plastic tubing from the stopper into a beaker, or small bucket, of water. This reaction will 
produce waste carbon dioxide and must be protected from air. The tubes in water allow the gas to 
escape while preventing any air from entering the bottle. 

The mixtures in the bottles are allowed to stand at room temperature until a lively evolution of 
gas starts, this will require from one to three hours. To the vigorously fermenting solutions add a 
total of 100 g of freshly prepared acetol; divide this equally between each bottle. The mixtures are 
allowed to stand at room temperature until the reaction subsides; adding the acetol may temporarily 
make it look like the reaction has subsided. The bottles are then transferred to a heated room kept at 
32 °C, where the fermentation continues. At the end of three days the reaction is generally 
completed. At this point the yeast is suction filtered using a pad of fiberglass or asbestos instead of 
filter paper. The filtrate is concentrated to a thick syrup under diminished pressure on a water bath, 
the temperature being kept below 40 °C. This can be a tricky to maintain the temperature. A handy 
way to regulate it is to start with only a small amount of filtrate in the flask, then connect an addition 
funnel to the distillation setup from which you add more cold filtrate over time. Control the rate of 
addition of the filtrate to maintain the optimal temperature. 

The residue (about 200 mL) is added to a mixture of 400 mL of anhydrous ethyl alcohol and 100 
mL of dry ether. The precipitate formed is removed by adding about 15 g of fiberglass fibers, 
stirring or shaking for 5 minutes, then suction filtering. The residue is extracted with a mixture of 
200 mL of 98.5% ethyl alcohol and 100 mL of dry ether. The combined alcohol-ether solutions are 
concentrated under diminished pressure at 35-40 °C to a thick syrup. The residue is again taken up 
in a mixture of 400 mL of 98.5% alcohol and 100 mL of dry ether, mixed with glass fibers, and 
suction filtered. The filtered liquid is concentrated under diminished pressure and distilled to obtain 
about 100 g of crude product. The crude material is redistilled and collected at 88-90 °C under 
vacuum or 187-189 °C under atmospheric pressure. The final product is a colorless liquid having a 
density near water. The yield is 49-58% or about 50-60 g. 



http://www.roguesci.org/megalomania/synth/synthesis4.html (14 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 



pyridine C 5 H 5 N 


1 


X 

W"/ ? x 

z 1 

uiMnown 


mp -41.6 bp 115.2 d0.98272 m79.10 


; $?.?? 


Safety Data: Flammable 


LASGUAiRD* I 
Storage Code 


Synonyms: 


Synthesis: Nothing yet 



silicic acid H 2 Si0 3 


1 


X 

W"/ ? N 

z 1 

unknown 


mp? bp ? ^ d? m? 


c $?.?? 


Safety Data: 


LABGUAF©* 

: Sloraqe Cods 

GREEN 


Synonyms: Dri-Die; precipitated silica; silica gel 


Synthesis: Nothing yet 



silver 


Ag 


1 


X 

W"/ ? N 

z 1 

unknown 


mp 960.5 bp 2000 d 10.49 


m 107.868 


c $?.?? 


Safety Data: 


jLABGUAflD* 
Storage Coda 

GREEN 




Synonyms: 


Synthesis: Nothing yet 



* 



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http://www.roguesci.org/megalomania/synth/synthesis4.html (15 of 16)12-8-2004 17:24:19 



Megalomania's Precursor Section Part 4 





http://www.roguesci.org/megalomania/synth/synthesis4.html (16 of 16)12-8-2004 17:24:19 




Megalomania's Precursor Section Part 1 



Precursors Part 1 



acetaldehyde 


CH3CHO 


LI #1 


O 


mp -123.5 bp 21 d 0.788 


m 44.05 


c $?.?? 






Safety Data: Flammable 


table key 


iLABGUAfiD* | 
[Storey Coae 


Synonyms: acetic aldehyde; acetylaldehyde; aldehyde; ethanal; ethyl aldehyde; ethylaldehyde 



Synthesis: Place 260 mL of 23% sulfuric acid in a 1500-mL dorence fl . Connect an addition 

funnel to the flask, and set it up for vacuum distillation with a 500-mL receiving flask. The 



receiving flask should be immersed in a salt-ice bath to cool the distillate when it comes over. 
Although a setup for vacuum distillation is used, it is not necessary to apply a vacuum; the vacuum 
adapter merely provides a means of equalizing pressure. Prepare a solution of 100 g of sodium 
dichromate in 200 mL of water and 127 mL of ethyl alcohol . Factor in the amount of water that is 
already in the ethyl alcohol when making the solution, i.e. 100 mL of 95% alcohol has 5 mL of 
water in it already. Place this solution in the addition funnel, position the stem of the funnel such 
that it is about 3 cm above the surface of the acid. Heat the acid until it just begins to boil, then add 
the mixture in the funnel in a steady stream to the acid. It will not be necessary to heat the flask 
during the addition because it will generate its own heat. The heat will be sufficient to distill over 
the acetaldehyde along with some alcohol and waste acetal. If acetaldehyde vapors begin to escape 
from the flask, regulate the distillation by decreasing the amount of dichromate solution being 
added. If the reaction flask does not boil on its own, gently heat it for a short time until boiling 
begins. 

The crude acetaldehyde thus obtained is difficult to distill from the alcohol and acetal mixed with 
it. It is therefore converted to aldehyde-ammonia, then back to pure aldehyde. Place the crude 
acetaldehyde in a Florence flask of suitable volume to contain no more than two thirds of the liquid. 
Attach a reflux condenser to the flask. Fill the condenser jacket with 30 °C water. It is only 
necessary to have the warm water in the jacket, not flowing. Stop up the lower connecter to prevent 
water from leaking out. To the top of the condenser, attach a glass tube connected to a wash bottle 
filled with 50 mL of ethyl ether . This wash bottle is then connected to another wash bottle filled 
with 50 mL of ether. After all connections have been made, the crude aldehyde is heated to a gentle 
boil for 5-10 minutes. The ether will absorb the acetaldehyde as it boils off. If the ether begins to 
rise up into the connecting tube from the condenser to the wash bottle, increase the heating. 





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Megalomania's Precursor Section Part 1 



Combine the ether into a 150-mL beaker immersed in a salt-ice bath. Bubble dry ammonia gas into 
the ether through an inverted funnel or wide tube immersed near the bottom of the beaker. Add 
ammonia until the ethereal solution smells strongly of ammonia. After about an hour, pure ammonia- 
aldehyde should have separated out. Scrape the crystals from the beaker and collect them by suction 
filtration. Wash the crystals with a small amount of ether, and allow them to dry in a desiccator. The 
yield is about 30 g. 

To obtain pure acetaldehyde, dissolve 10 g of aldehyde-ammonia in 10 mL of water in a 50-mL 
Florence flask. Add 28 mL of cold 29% sulfuric acid to the flask and set it up for simple distillation. 
Heat the flask on a water bath to distill over the aldehyde. Place the receiving flask in a salt-ice bath 
to cool the volatile acetaldehyde. 

Acetaldehyde is extremely volatile and cannot be stored satisfactorily unless it is refrigerated or 
sealed in glass ampoules (not just capped), therefore it is necessary to prepare acetaldehyde each 
time it is needed. There is, however, an easier solution. A quick and easy way to store acetaldehyde 
is to polymerize it to paraldehyde, which can be handled and stored easily, then depolymerize when 
you need to use it. Now you can make a larger amount without worry. 

To polymerize acetaldehyde for storage, place it in a dry test tube and cautiously add 1 drop of 
concentrated sulfuric acid per 2 mL of acetaldehyde in the tube. Mix thoroughly, the polymerization 
will begin to take place. Some gentle warming can hasten the reaction. After some minutes add 3-4 
mL of water per 2 mL of acetaldehyde, an insoluble precipitate of paraldehyde will form. As an 
aside, technically paraldehyde is a controlled substance. It is a sedative and a hypnotic drug useable 
by prescription only. 

To depolymerize paraldehyde back into acetaldehyde, place the paraldehyde into a round-bottom 
200-mL Florence flask. Add 4-5 drops of concentrated sulfuric acid for every 20 g (20 mL) of 
paraldehyde in the flask. Set the flask up for fractional distillation, use glass in the fractionating 
column. Use a 125-mL Erlenmeyer flask as the receiver; keep it cool by immersing in an ice water 
(but not salt-ice) bath. Place a loose plug of cotton into the Erlenmeyer flask to help reduce 
evaporation loss; it must be loose. Care must be taken to prevent the cotton from coming into 
contact with the distillate. After setting up, heat the flask gently. The temperature of the distillate 
must not be allowed to rise above 35 °C as it will only repolymerize. The acetaldehyde is now ready 
for use. 



acetamide 


CH 3 CONH 2 


L2 #1 


0 


mp 81 bp 222 d 1.159 


m 59.07 


c $?.?? 


Safety Data: 


jLABGUARD* 
j Siorage Code 

GREEN 




Synonyms: acetic acid amide; acetimidic acid; ethanamide; methanecarboxamide 



http://www.roguesci.org/megalomania/synth/synthesisl.html (2 of 24)12-8-2004 17:24:27 



Megalomania's Precursor Section Part 1 



Synthesis: Place 71.5 mL of glacial acetic acid into a ceramic or porcelain dish, heat the acid to 

40-50 °C by a water bath. Neutralize the acid by adding 100 g of finely pulverized ammonium 
carbonate ; the resulting compound should be slightly alkaline. The mass is warmed on the water 
bath to 80-90 °C until acidic, test for acidity by adding a few drops to a test tube of water then drop 
on litmus or pH paper. 

The reaction is now completed in a bomb tube, or Volhard tube, this is essentially a glass bottle 
that is sealed by melting the glass together at the opening. Since these may be hard to come by a 
substitute is needed. A heavy walled glass beer or wine bottle should lend itself well to acting as a 
reaction container. There is a strong possibility that such a bottle can burst under the great heat 
required of this reaction, this applies to the Volhard tube as well. The tube or bottle should be 
wrapped in a fine mesh metal screen, the kind used on windows, if it bursts the screen will prevent 
glass going everywhere. Heating the tube behind a sheet of wood is also a good idea. 

It will be quite necessary to melt the top of the glass closed; using a mere rubber or cork stopper 
is not sufficient because they will melt or burn. To seal the open end of a tube charged with the 
substance, it is warmed by holding it at an angle of about 45°, with constant turning, in the small 
luminous flame of a burner, and then heated strongly in the larger non-luminous flame. Heat the 
neck if using a bottle. When the glass becomes soft, use pliers to gently pull and squeeze the top of 
the tube upwards causing the glass of the neck to narrow. Continue to heat this narrowed portion 
and draw the top up until the glass has closed itself off. After breaking off or cutting of the end of 
the tip, to allow the air to escape on further heating, it is heated just below the top. When the tube is 
softened at this point it is drawn out slightly, heat is applied just below the top, it is drawn out again, 
and so on. The result is that the form of the top of the tube gradually changes from a cylinder to a 
sharp-pointed cone. The narrowest part of the cone is then heated without drawing it further. The 
soft glass melts together, and a thick walled cap is obtained. 

Fill the tube, previously heated by flame, with the compound while hot without using a funnel. If 
any portion adheres to the top of the tube, melt it down by carefully heating with a flame. Any 
remaining trace can be wiped away, now seal the tube as described above. Heat the tube for 5 hours 
at 220-230 °C in a furnace. After heating, break the bottle open to obtain the reaction product. The 
liquid product is fractionally distilled in a well ventilated area. The first fraction that distills over 
between 100-130 °C will be acetic acid and water. The temperature will then rise rapidly to 180 °C 
where upon acetamide will begin to distill over. Collect the portion distilling over between 180-230 ° 
C in a beaker. Cool the beaker with a salt-ice bath towards the end of the distillation. Rub the walls 
of the beaker after the distillation to crystallize the impure acetamide. The crystals are placed on a 
Buchner funnel and pressed to squeeze out any liquids. The crystals are now simple distilled to 
obtain almost pure acetamide. To remove the last traces of impurities, again press the crystals, then 
recrystallize from a minimum amount of ethyl ether . Filter to collect the crystals, allow a brief 
period to dry. Yield is about 40 g. 



acetic acid 



CH 3 COOH 



http://www.roguesci.org/megalomania/synth/synthesisl.html (3 of 24)12-8-2004 17:24:27 



Megalomania's Precursor Section Part 1 



mp 16.7 


bp 118 




d 1.0492 


m 60.05 


c $?.?? 




Safety Data: Corrosive, Flammable 

JS M 


LABGUARD* 
Storage Code 

WHITE 





Synonyms: acetate; acetic acid glacial; Aci-Jel; ethanoic acid; ethylic acid; glacial acetic acid; 
methanecarboxylic acid; shotgun; TCLP extraction fluid 2; vinegar; vinegar acid 



Synthesis: Acetic acid is available as an OTC chemical in the form of vinegar, a dilute solution of 

acetic acid. Vinegar should be available from any grocery story in 3%-5% concentrations or so. 
Acetic acid is a chemical that I consider to plentiful to bother synthesizing yourself since it is a 
cheap, abundant OTC chemical. It can be done, and it may be cheaper in the long run to make it on 
your own, but I do not have the information handy. A trip to the library, or a web search will yield 
much info on the topic. Acetic acid is more useful in concentrated, or glacial, form. Only acetic acid 
is referred to as glacial rather than concentrated acid. This is because the ancients liked how much 
frozen acetic acid looked, it reminded them of an ice glacier, so the term glacial stuck. Glacial acetic 
acid is very corrosive and slightly flammable. 

Vinegar can be made into glacial acetic acid by first converting it to sodium acetate . Once you 
have some sodium acetate ready, set up the necessary equipment for a simple distillation and fill the 
reaction flask with concentrated (95%+) sulfuric acid . Add the sodium acetate to the acid and begin 
the distillation. The sulfuric acid will break down the sodium acetate and the resulting acetic acid 
will distill off. The concentration of the acetic acid obtained will be nearly anhydrous, especially if 
you start with thoroughly dried sodium acetate and 100% sulfuric acid. 



acetic anhydride 


(CH 3 C0) 2 0 


mp -73 


bp 139 


d 1.080 


m 102.09 



Safety Data: Corrosive, Flammable 




Synonyms: acetic acid anhydride; acetic oxide; acetyl anhydride; acetyl ether; acetyl oxide; 
ethanoic anhydrate; ethanoic anhydride 



http://www.roguesci.org/megalomania/synth/synthesisl.html (4 of 24)12-8-2004 17:24:27 



Megalomania's Precursor Section Part 1 



Synthesis: Acetic anhydride is a very handy organic compound that has fallen into ill repute 

thanks to the drug dealers. It is technically a watched chemical, but you will only have to answer 
questions at gunpoint if you buy over 250 gallons. Even so, you will most likely be put on The List 
if you buy any, and you will have to come up with a bunch of explanations as to what you are going 
to do with it. Acetic anhydride is very corrosive and must be kept away from moisture, as it will 
decompose into acetic acid. 

Into a 200-mL Florence flask, add 70 g of finely pulverized, anhydrous sodium aceta . Set the 
flask up for simple distillation, instead of a thermometer in the top of the flask use an addition 
funnel. Slowly add, by drop wise addition, 45.5 mL of acetyl chloride from the addition funnel. After 
half of the acetyl chloride has been added, stop the addition and stir the reaction mix with a glass 
stirring rod. Afterwards, continue the addition the rest of the way. If at any point during the addition 
some material should distill over, pour it back into the reaction flask and decrease the rate of 
addition to prevent this. After the addition is complete, remove the addition funnel, stop up the 
flask, and distill with flame or hot plate. The crude acetic anhydride thus obtained needs to be 
purified by distillation. Set up for a simple distillation, add 3 g of finely pulverized, anhydrous 
sodium acetate to the reaction flask, and then pour in the crude acetic anhydride. The sodium acetate 
will convert any remaining acetyl chloride into the anhydride. The receiving flask should be under a 
water shower for cooling. Place a large funnel (a cheap plastic one will work fine) under the flask 
with a tube leading to the sink, pour cold water over the top of the receiving flask. The receiving 
flask can also be held directly under the faucet in the sink. Commence the distillation; the yield 
should be about 50 g of pure acetic anhydride. 



acetone 


CH3COCH3 


5 


0 


mp -94 


bp 56.5 


d 0.788 


m 58.08 


c $?.?? 


Safety Data: Flammable 




LABGUARD* 
StO-at-iB Cot: ft 





Synonyms: 2-propanone; chevron acetone; dimethyl formaldehyde; dimethylketal; dimethyl 
ketone; ketone propane; beta-ketopropane; methyl ketone; propanone; pyroacetic acid; pyroacetic 
ether 



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Megalomania's Precursor Section Part 1 



Synthesis: Acetone is available as an OTC chemical in just about every hardware store. The stores 

sell it cheap, pure, and in large quantities. As far as Synthesis goes it is rather complicated, so it is 
best to purchase it. Its primary use in the household is as a solvent for paint, i.e. thinning paint, 
removing varnishes, and cleaning brushes. It can be purchased in pint to 5-gallon sizes at hardware 
stores or paint supply stores without question. 

Acetone can be dried out by adding a small amount of calcium chloride , say 1 g per 25 mL, and 
letting it stand for three to seven days in a sealed container. Occasional agitation, every 12-24 hours, 
will improve the drying process. After letting the acetone stand, distill it to get the dry acetone. 

Some of the acetone will combine with the calcium chloride, so it necessary to distill it. Store the 
dry acetone in a well-sealed container. 



acetyl chloride 


CH 3 COCI 


6 






mp -112 


bp 52 


d 1.104 


m 78.50 


; $?.?? 


C 


D 










LABGUAiRD* 1 






Safety Data: MSDS 






S.I.O'jrje Cot: ft 




^Cl 


Synonyms: acetic acid chloride; acetic chloride; ethanoyl chloride 



Synthesis: Place 95 mL of glacial acetic acic into a round-bottomed 500-mL Florence flask. Set 

the flask up for vacuum distillation with addition. Instead of connecting the vacuum adapter to a 



vacuum source, attach a calcium chloride drying tube. There is no need for vacuum, just an airtight 
connection to protect the product from moisture. While cooling the flask in a salt-ice bath, slowly 
add 51 mL of )hosphorus trichloride through the addition funnel. After the addition, place the flask 
in a water bath heated to 40-50 °C. Continue heating until the active evolution of hydrochloric acid 
gas slackens, and the liquid separates into two layers. 

To separate the acetyl chloride, which should have formed on the upper layer, heat the flask on a 
boiling water bath until nothing more distills over. To purify the acetyl chloride, simple distill the 
product obtained in the same apparatus used before, except this time replace the addition funnel 
with a thermometer. Collect the portion distilling over from 50 to 56 °C. The yield is about 80-90 g. 



acrylic acid 


ch 2 =cfico 2 h 


7 


mp 14 


bp 141.0 


d 1.0621 


m 72.06 


c $?.?? 



Safety Data: Corrosive, Flammable 



LABGUARD* 
Storage Code 

WHUE 




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Megalomania's Precursor Section Part 1 





Synonyms: 2-propenoic acid ; acroleic acid; acrylate; ethylenecarboxylic acid; propene acid; 
propenoic acid; vinylformic acid 




Synthesis: Prepare a mixture of 151 mL of 98-100% formic acid, 1060 mL of methyl acrylate, 30 

g of hydroquinone, and 2 mL of Ifuric acid in a round-bottomed 2-L flask. Set the flask up for 
refluxing. Reflux with an oil bath heated to 85-95 °C (the oil not the contents of the flask) for 1-3 
hours. 

Remove the reflux column and set the flask up for fractional distillation, using copper sponge to 
pack the column. Slowly distill the mixture at 32-35 °C for about 8-10 hours, you will be removing 
methyl formate waste from the mixture. You will want to let 1 drop of distillate come over for every 
5 that fall back into the flask, then allow more to come over near the end. 

When no more methyl formate is produced, the excess methyl acrylate is fractionally distilled 
under partial vacuum at 32-35 °C with the oil temperature at 60-65 °:C. Reconfigure the setup for 
vacuum distillation if need be. You will also need to add a clasien adapter so as to extend a length of 
tubing into the mixture. During the distillation, a slow stream of carbon dioxide is admitted through 
this tube. 

When all the methyl acrylate has been removed, the acrylic acid is fractionally distilled at 53-56 ° 
C under vacuum. Upon redistillation acrylic acid of 97% purity is obtained in a yield of 74-78% or 
about 220-230 g. 



acrylyl chloride H 2 C=CHC0C1 


8 


O 


mp? bp 72-76 d 1.1140 m 90.51 


; $?.?? 


Safety Data: Corrosive, Flammable 


LABGUARD* 1 
StO’-aoH Col: e 


Synonyms: acryl chloride; acrylic acid chloride; acryloyl chloride; chlorid kyseliny akrylove; 2- 
propenoyl chloride; propenoyl chloride 



Synthesis: Into a 1-L round-bottomed flask place 135 mL of thionyl chloridt . Set this flask up for 

refluxing with addition. Heat the thionyl chloride to boiling, and then add 115 mL of lie acid at 
such a rate that the mixture refluxes gently. It may require about an hour to add all of the acid. This 
reaction will generate toxic sulfur dioxide gas, so take the necessary precautions. After all of the 
acid has been added, continue to reflux for an additional 30 minutes to expel all of the sulfur dioxide 
gas. 

I have no information on how to isolate or purify this chemical. It will be mixed with 
hydrochloric acid as a waste byproduct. I would suggest neutralizing the acid by adding some 
sodium hydroxide, and then distilling the product to get pure acrylyl chloride. If using this chemical 
to make l,l,l-trinitro-2-propyl acrylate, try using aluminum hydroxide to neutralize the acid. The 
product of this is aluminum chloride, which is needed in the reaction, so no need to distill this. 



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Megalomania's Precursor Section Part 1 



allyl methanesulfonate 


c 4 h 8 o 3 s 


9 




mp ? bp ? d W 


m 136.1 


c$?.?? 


/ ch 4 


Safety Data: 


ChemAlcn* 
Sic rage Coda 

Oft AY 





Synonyms: allyl mesylate; methanesulfonic acid, allyl ester; methanesulfonic acid, 2-propenyl ester 



Synthesis: In a 1000-mL Erlenmeyer flask prepare a solution of 20 g of distilled allyl alcohol 

(98%) in 300 mL of diethyl ether. Cool the flask in an ice-water bath to below 5 degrees C. With 
stirring add 56.5 g of solid potassium carbonate in one portion; next add 3.3 g of solid 
trimethylamine hydrochloride in one portion. Stir the resulting suspension for 5 minutes. With 
vigorous stirring add 46.9 g of methanesulfonyl chloride to the flask dropwise over a period of 1 
hour. After the addition of methanesulfonyl chloride is complete continue stirring the contents of the 
flask for 5 hours and maintain the temperature at 5 degrees C. Next add 300 mL of water to the flask 
and continue to stir the contents vigorously for an additional 15 minutes before discontinuing the 
stirring. Allow the contents of the flask to separate into two layers, the aqueous layer will be on the 
bottom. Decant off as much of the aqueous layer as possible by a pipette and collect it in a separate 
beaker. Mix the aqueous portion with two portions of 100 mL of ethyl ether and shake them in a 
seperatory funnel. It may be necessary to break up the aqueous layer into four batches to fit into the 
seperatory funnel, in which case shake each 75 mL portion of water with two 25 mL portions of 
ether. Combine all of the ether extracts with the organic layer in an Erlenmeyer flask and add a 
portion of anhydrous magnesium sulfate to draw out any moisture. Remove the ether by evaporating 
under reduced pressure without heating. The remaining allyl methanesulfonate is poured over a 
filter to remove the magnesium sulfate and kept under high vacuum to remove any final traces of 
solvent. What remains should be about 38-39 g of clear colorless oil. Yield is 83%. If possible this 
reaction should be carried out under an atmosphere of nitrogen. 



A 



aluminum 


A1 


10 


Al 


mp 660 bp 2327 d 2.70 


m 26.981539 


: $?.?? 


Safety Data: Flammable 


LABGUAflD* 


Synonyms: aluminium 



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Megalomania's Precursor Section Part 1 



Synthesis: Aluminum powder will add explosive strength to just about any high explosive. The 

powder only that is, not foil or wire. The kind of powder needed is very finely divided, not the kind 
that can be purchased from automotive stores as a leak plugger for the radiator, that variety is too 
coarse. The only possible OTC source is from paint stores as an additive for paint. I should mention 
that I have never seen it sold in paint stores. 

If all else fails one can buy finely powered aluminum from chemical suppliers who deal with the 
public. Companies that sell pyrotechnic materials will in all likelihood have several grades available 
from coarse down to atomized. 

When using aluminum in chemical reactions one can use aluminum foil available at any grocery 
store, or aluminum tubing or rod available at hardware stores. Aluminum products are quite 
abundant at many stores. Aluminum foil is quite versatile because it offers a higher surface area 
compared to other types of OTC aluminum, it is quite cheap, and is pure. Aluminum foil is easy to 
tear into a desired mass and can be crumpled into balls of any size if coarse bits are needed for a 
reaction. Aluminum tubing or rod will need to be machined to get turnings, chunks, or shot which 
sounds like a lot work and special equipment. 



aluminum chloride 


A1C1 3 


11 


Cl 

cr ci 


mp ? 


bp ? 


d? 


m 133.34 


c $?.?? 


Safety Data: Corrosive 


labguard* 
Storage Code 

WHITE 




Synonyms: A1C13; alluminio(cloruro di); aluminiumchlorid; aluminium, (chlorure d'); aluminium 
trichloride; aluminum chloride (1:3); chlorure d'aluminium; Drysol; NSC 143016; PAC (salt); 
Pearsall; trichloroaluminum; UN 1726; UN 2581 



Synthesis: The Synthesis of aluminum chloride will require a creative glassware setup. Assemble 

a heating apparatus as shown in the illustration below; each part must be completely dry for the 
reaction to work. The long furnace tube of hard glass should be 1.5 to 2 cm in diameter. The length 
is up to you, but a tube of 25-40 cm should suffice. One end of the tube can be drawn out to a 
narrow aperture if desired, since that requires some glassblowing skill it may be difficult for the 
improviser. A stopper with a short length of glass tubing in the middle will do nicely. The wide end 
of the tube is inserted into the center of a large stopper, a second glass tube, of at least 8 mm 
diameter, bent at a right angle, is placed above the larger. The large stopper is then attached to a 
wide mouth glass bottle. The part of the tube extending beyond the flames must be as short as 
possible to prevent the product from condensing prematurely, or it will clog the tube. Each end of 
the tube is plugged with glass wool to keep the reactants inside. A heat resistant plate is secured 
between the bottle and the flame to protect the stopper from burning or melting, you can use glass 
wool, aluminum foil, or any kind of fire resistant material (asbestos was recommended, it is now 
unavailable). If you have a stopper at the other end instead of a narrowed end, you will need a plate 



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Megalomania's Precursor Section Part 1 

there too. Fill the glass tube half way (horizontally, not vertically) with aluminum shavings before 
assembling of course. You can use little aluminum foil balls, or machine shop shavings, the latter 
must be cleaned of oil by boiling in ethyl alcohol and dried in an oven at 120 °C. 

A very rapid current of dry ogen chloride gas is passed into the tube from the narrow end; 
the gas first passes into two drying bottles filled with concentrated sulfuric acid . Do not fill the 
bottles with too much acid as it can foam up. Test to see if all of the air has been removed from the 
apparatus by connecting a rubber hose to the angled outlet tube and directing the gas into a beaker 
of water. When only HC1 gas remains, it will be absorbed directly into the water with little or no 
bubbling, now remove the tubing. If any air remains, there can be an explosion of oxygen and 
hydrogen. Now that the air is out, begin heating the tube with several burners along its length. Start 
with small flames and gradually increase. White vapors of aluminum chloride will begin to be 
evolved when the flames are high enough, and will be condensed into the bottle. Do not heat the 
aluminum so high it melts, if this happens remove the flames immediately. Continue heating when it 
solidifies. The reaction is done when all of the aluminum has been consumed, a small amount of 
dark residue may remain. The current of hydrogen chloride gas must be kept constantly rapid for 
this reaction to work. The aluminum chloride thus obtained is quite pure; store it in tightly sealed 
bottles or a desiccator. 



aminoguanidine bicarbonate 


c 2 h 8 n 4 o 3 


12 


mp ? bp ? d ? 


m ? 


c $?.?? 


Safety Data: Irritant 


j l^bguahd* 

| Storage Coda 

GREEN 





HO 



NH 



/ 



■OH H 2 N_ 



>T 

H 



'HH, 



Synonyms: aminoguanidinium hydrogen carbonate; carbonic acid with hydrazinecarboximidamide 

( 1 : 1 ) ' 



Synthesis: Two hundred and sixteen grams (2.07 moles) of nitroguanidinel and 740 g. (1 1.3 

moles) of purified zinc dust (Note 1) are thoroughly ground together in a mortar, and then enough 
water (about 400 ml.) is added with stirring with the pestle to form a thick paste. The paste is 
transferred to a 3-1. enameled can or beaker surrounded by an ice bath. A solution of 128 g. (2.14 
moles) of glacial acetic acid in 130 ml. of water is cooled to 5° in another 3-1. beaker, which is fitted 
with a strong mechanical stirrer and surrounded by an ice bath. The paste of nitroguanidine and zinc 
dust, cooled to 5°, is added slowly with mechanical stirring, the temperature of the reaction mixture 
being kept between 5° and 15°. A total of about 1 kg. of cracked ice is added to the mixture from 
time to time as the mixture becomes too warm or too thick to stir. The addition of the paste takes 
about 8 hours, and the final volume of the mixture is about 1.5 1. (Note 2). The mixture is then 
slowly warmed to 40° on a water bath with continued stirring, and this temperature is maintained for 
1-5 minutes, until reduction is complete (Note 3). 



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Megalomania's Precursor Section Part 1 



The solution is immediately separated from the insoluble material by filtration on a 20-cm. 
Buchner funnel, and the cake is sucked as dry as possible. The residue is transferred to the 3-1. 
beaker, triturated well with 1 1. of water, and then separated from the liquid by filtration. In the same 
manner, the residue is washed twice more with two 600-ml. portions of water. The filtrates are 
combined and placed in a 5-1. round-bottomed flask. Two hundred grams of ammonium chloride is 
added, and the solution is mechanically stirred until solution is complete (Note 4). The stirring is 
continued, and 220 g. (2.62 moles) of sodium bicarbonate is added during a period of about 10 
minutes. The aminoguanidine bicarbonate begins to precipitate after a few minutes, and the solution 
is then placed in a refrigerator overnight. The precipitate is collected by filtration on a Buchner 
funnel. The cake is removed to a 1-1. beaker and mixed with a 400-ml. portion of a 5% solution of 
ammonium chloride and filtered. It is again washed with two 400-ml. portions of distilled water, the 
wash solution being removed each time by filtration. Finally the solid is pressed down on the 
Buchner funnel; the mat is broken up with a spatula and washed while on the funnel with two 400- 
ml. portions of 95% ethanol and then with one 400-ml. portion of ether. After air drying, the 
aminoguanidine bicarbonate amounts to 180-182 g. (63-64%) of a white solid, melting at 172° with 
decomposition (Note 5) and (Note 6). 

1. The zinc is purified by stirring 1.2 kg. of commercial zinc dust with 3 1. of 2% hydrochloric 
acid for 1 minute. The acid is removed by filtration, and the zinc is washed in a 4-1. beaker with one 
3-1. portion of 2% hydrochloric acid, three 3-1. portions of distilled water, two 2-1. portions of 95% 
ethanol, and finally with one 2-1. portion of absolute ether, the wash solutions being removed each 
time by filtration. Then the material is thoroughly dried and any lumps are broken up in a mortar. 

2. The solution becomes basic to litmus after one-half to three-fourths of the paste has been 
added. Lower yields are obtained if a larger excess of acetic acid is employed. 

3. The state of reduction can be determined by placing 3 drops of the reaction mixture in a test 
tube containing 5 ml. of a 10% solution of sodium hydroxide and then adding 5 ml. of a freshly 
prepared saturated solution of ferrous ammonium sulfate. A red coloration indicates incomplete 
reduction; when the reduction is complete, only a greenish precipitate is observed. The mixture 
should not be heated after this test shows that reduction is complete. 

4. The presence of the ammonium chloride prevents the coprecipitation of zinc salts when 
sodium bicarbonate is added to the solution to precipitate the aminoguanidine as the bicarbonate. If 
the solution is not clear at this step, it should be filtered. 

5. The aminoguanidine bicarbonate is pure enough for most purposes. It should not be 
recrystallized from hot water, since decomposition will occur. 

6. W. W. Hartman and Ross Philips have submitted a procedure suitable for the preparation of 
aminoguanidine bicarbonate on a larger scale. The sulfates of methylisothiourea and of hydrazine 
are allowed to react with the evolution of methyl mercaptan. In a 30-gal. crock are placed 10 1. of 
water and 5760 g. (20 moles) of methylisothiourea sulfate. 2 In a 22-1. flask, 5.2 kg. (40 moles) of 
hydrazine sulfate3 is stirred with 12 1. of water, and 40% sodium hydroxide is added until all the 
hydrazine sulfate has dissolved and the solution is just neutral to Congo paper. The exact amount of 
alkali is noted and a duplicate amount added. The hydrazine solution is then added to the 30-gal. 
crock with stirring, as fast as possible, without allowing the foam to overflow the crock. The mixing 
is done out-of-doors, or in an efficient hood, since large volumes of methyl mercaptan are evolved. 



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Megalomania's Precursor Section Part 1 



If the reaction is carried out on a smaller scale in 12- or 22-1. flasks, using appropriate amounts of 
material, the methyl mercaptan evolved may be absorbed in cold sodium hydroxide solution and 
isolated if desired. The solution is stirred until evolution of mercaptan stops, and then a few liters of 
water are distilled off under reduced pressure to free the solution entirely from mercaptan. The 
residual liquor is chilled in a crock, and a crop of hydrated sodium sulfate is filtered off, washed 
with ice water, and discarded. The filtrate is warmed to 20-25°, 25 ml. of glacial acetic acid is 
added, then 4 kg. of sodium bicarbonate, and the solution is stirred vigorously for 5 minutes and 
thereafter occasionally during an hour, or until the precipitate no longer increases. The precipitate is 
filtered with suction and washed with ice water and then with methanol, and is dried at a 
temperature not above 60-70°. The yield is 3760 g. (69% of the theoretical amount). Hydrazine 
sulfate may be recovered from the final filtrate, if the filtrate is strongly acidified with sulfuric acid 
and allowed to cool. 

This procedure borrowed from Organic Synthesis Collective Volume 3 pg 73 



ammonia NH 3 


13 




mp -77.7 bp -33.35 d 0.6818 m 17.03 


c $?.?? 


Safety Data: Corrosive, Irritant, Toxic 


i LABGUARD" 

| Storage? Code 




M 


BLUE 


Synonyms: N-H 



Synthesis: One method gaseous ammonia can be generated is by heating a small flask full of the 



most concentrated ammonium hydroxide available with a burner, household hydroxide will not be 
sufficient. The gas can be dried by passing it through a drying tube filled with a mixture of 4 parts 
calcium oxide with 1 part sodium hydroxide. 



ammonium carbonate 


(NH 4 ) 

2 C0 3 


14 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 




j LABGUARD* 

| Storage Code 






GREEN 



TT 



M+. 

' S^"H 

TH 



w+. 

- N^'h 

OH 



Synonyms: ammonium sesquicarbonate; carbonic acid, ammonium salt; carbonic acid, 
diammonium salt; crystal ammonia; diammonium carbonate; hartshorn 



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Megalomania's Precursor Section Part 1 



Synthesis: Coming soon! 



ammonium chloride 


NH 4 C1 


15 


cr 

H 

"A" 


mp ? bp ? d 1.5274 


m 53.49 


c $?.?? 


Safety Data: MSDS 


jLABGUAfiD* 
Storage Code 

GREEN 




Synonyms: Amchlor; ammoneric; ammoniumchlorid; ammonium muriate; chlorid amonny; 
Darammon; sal ammonia; sal ammoniac; salammonite; salmiac 


Synthesis: Coming soon! 









(NH 4 ) 2 Fe 


ammonium ferrous sulfate 


(S0 4 ) 2 • 








6 H 2 0 


mp 100 
(dec) 


bp- 


d 1.86 


m 284.05 



-Q 



Fe' 1 



□ 

S O- 

□ 

NH*' 

□ nh; 



Safety Data: DS 



] L^BGUAHD* 

: Storage Code 

green' 




Synonyms: ammonium iron sulfate; ferrous ammonium sulfate; iron ammonium sulfate; Mohr's 
salt; sulfuric acid, ammonium iron(2+) salt 



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Megalomania's Precursor Section Part 1 



Synthesis: Prepare a solution of 234 g of ammonium bisulfate in 1 L of water. Add 42.7 g iron 

metal to the solution and heat to 70 degrees C until all of the iron dissolves (reacts). Add an 
additional 234 g of ammonium bisulfate to the solution and again add 42.7 g of iron and heat to 70 
degrees until all of the iron reacts. Cool the solution down to less than 15 degrees C with stirring; 
ammonium ferrous sulfate should then precipitate. Pour the liquid over a filter to collect the crystals. 
You may need to boil the liquid down to half its volume to obtain a complete crop of crystals. 

The ammonium bisulfate used in this reaction can be obtained by heating ammonium sulfate to 
370 degrees C and cooking for about 15-20 minutes. Ammonium sulfate can be obtained either as 
fertilizer or by reacting ammonia with sulfuric acid. 



ammonium hydroxide 


NH 4 OH 


17 


mp - bp - d 0.90 


m - 


c $?.?? 


Safety Data: Corrosive 


LABGUARD* 
Storage Code 

WHFTE 





Synonyms: ammonia, monohydrate; ammonia water; ammonium, aqueous; aqua ammonia; aqueous 
ammonia; Spirit of Hartshorn 


Synthesis: Coming soon! 






aniline 


c 6 h 5 nh 2 


18 




nh 2 


mp -6 bp 184-186 d 1.022 


m 93.13 


c $?.?? 




Safety Data: Toxic 


LABGUARD' 
Storage Code 

BLUE 





Synonyms: benzamine\ aminobenzene; aminophen; anilin; anilina; aniline oil; aniline reagent; 
anyvim; arylamine; benzene, amino-; benzidam; blue oil; C.I. 76000; C.I. oxidation base 1; cyanol; 
Huile D'aniline; krystallin; kyanol; NCI-C03736; phenylamine; Rcra waste number U012; UN 1547 



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Megalomania's Precursor Section Part 1 



Synthesis: Prepare a mixture of 90 g of tin granules and 41.5 mL of nitrobenzene in a round 

bottom 1500-mL flask. Gradually add about 17 ml of concentrated hydrochloric acid , attach a reflux 
condenser, with or without water flowing, and shake the flask until thoroughly mixed. The flask will 
become warm after a short time, and a vigorous reaction can be observed. When this happens, 
immerse the flask in cold water to moderate the reaction. Add another 17 mL of hydrochloric acid 
and repeat the shaking/cooling process. Add a third and fourth portion of acid until approximately 
80-85 mL of acid has been added, shaking and cooling each time. At this point the addition of acid 
should not give as quite a violent reaction, add an additional 85-90 mL of hydrochloric acid in larger 
portions. The total amount of acid added is 167 mL. 

After all of the acid has been added, the mixture is heated on a steam bath for 1 hour at reflux. 
After refluxing, add 100 mL of water to the flask. Prepare a solution of 150 g of sodium hydroxide 
in 200 mL of water, gradually add this solution to the flask in small portions. If the addition of the 
hydroxide solution causes the contents of the flask to boil, cool the flask in a water bath before 
adding more. 

To distill the aniline, set the flask up for steam distillation and distill, aniline and water will be 
collected. The initial distillate will be a milky color, when it becomes clear remove the collecting 
flask and add a new one. Collect an additional 300 mL of distillate. 

Combine the two distillate portions in an Erlenmeyer flask, and then add 25 g of finely powdered 
sodium chloride for every 100 mL of distillate collected. Shake the flask until all of the salt 
dissolves, then extract the solution with several portions of ether . Combine the ether portions, add a 
small amount of )otassium hydroxide , and allow the ether to evaporate. The crude aniline thus 
obtained can be purified by simple distillation. The yield is 90-100%. 









CfTLN. 


aniline hydrochloride 


HC1 


mp 198 


bp 245 


d 1.2215 


m 

129.5889 



Safety Data: MSDS 




Synonyms: aniline chloride; aniline hydrochloride; aniline salt; anilinium chloride; benzenamine 
hydrochloride; C.I. 76001; hydrochloride benzenamine; phenylamine hydrochloride; 
phenylammonium chloride 



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Megalomania's Precursor Section Part 1 



Synthesis: Aniline hydrochloride is made by gradually adding concentrated hydrochloric acid to 
aniline. One method to test for completion is by placing a drop of solution on a piece of filter paper 
stained with methyl violet. If it turns green it is done. Otherwise add an excess of hydrochloric acid. 
After the acid has been added, cool the solution rapidly, with stirring, by placing it in a salt-ice bath. 
Small crystals of aniline hydrochloride will precipitate. Vacuum filter the solution to collect these 
crystals, press them with filter paper to squeeze out any excess water, and allow to dry. 





aspirin C 9 H 8 0 4 


18 


o on 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: 


.] LABGUAR D* 

| Siorage Code 

GREEN 


Synonyms: 2-(acetyloxy)-benzoic acid ; ac 5230; acenterine; acesal; Acetaminophen Aspirin; 
acetate salicylic acid; aceticyl; acetilsalicilico; acetilum acidulatum; acetisal; acetonyl; acetophen; 
acetosal; acetosalic acid; acetosalin; 2-acetoxybenzoic acid; acetylin; acetylsal; acetylsalicylic acid; 
acetyl salycylic acid; acidum acetylsalicylicum; acimetten; acisal; acylpyrin; Alka-seltzer; Anacin; 
A.S.A.; a.s.a. empirin; asagran; asatard; Ascoden-30; Ascriptin; aspalon; aspergum; aspirdrops; 
Aspro; asteric; benaspir; bialpirinia; Bufferin; caprin; o-carboxyphenyl acetate; Chlorpheninaurine; 
colfarit; contrheuma retard; Coricidin; Coricidin D; cr; Darvon compound; duramax; ECM; Ecotrin; 
empirin; endydol; entericin; enterosarine; entrophen; Excedrin; extren; Gelprin; helicon; Measurin; 
Norgesic; Persistin; rhodine; Robaxisal; salacetin; salcetogen; saletin; salicylic acid acetate; Supac; 
Triaminicin; Vanquish; XAXA 


Synthesis: Coming soon! 



barium chloride 


BaCl 2 


19 


cr 03 ++ cr 


mp 963 bp - d 3.86 


m 208.23 


c $?.?? 


Safety Data: Toxic 


LA8GUARD* 
Storage Code 

BLUE 




Synonyms: ba 0108E; barium dichloride; NCI-C61074; SBA 0108E 


Synthesis: Coming soon! 



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Megalomania's Precursor Section Part 1 



benzal chloride 


C 6 H 5 CHC1 2 


20 


c, c, 


mp -17 bp 205 d 1.26 


m 161.03 


c $?.?? 


Safety Data: MSDS 


LAEiGUARD" 
Storage? Code 

BLUE 


Synonyms: benzylidene chloride; (dichloromethyl)benzene; benzyl dichloride; benzylene chloride; 
benzylidene dichloride; chlorobenzal; dichloro methyl-benzene; a,a-dichlorotoluene; 
dichlorophenylmethane 



Synthesis: Place 58 mL (50 g) of toluene in a round bottom 100-mL flask. Attach a Clasien 

adapter to the flask. On the angled arm of the adapter, attach a condenser set up for refluxing. Since 
excess chlorine gas will be released from the top of the condenser, affix a one-holed stopper with a 
short length of glass tubing connected to a long hose, direct the hose to a well ventilated area. On 
the straight arm of the adapter, attach a length of glass tubing with a bubbler at the end that extends 
below the surface of the toluene. The top of this tube is connected to a chlorine generator. 

Position the setup such that the flask is in direct sunlight, or very strong light. Sunlight is 
superior. Heat the toluene to boiling while a current of dry chlorine gas is bubbled in, the chlorine 
can be dried by passing it through two drying bottles filled with concentrated sulfuric act . The 
course of the reaction is best judged by weighing the product; the reaction is complete when the 
toluene has increased by 40 g, the total weight being 90 g. By weighing the flask beforehand, and 
periodically interrupting the flow of chlorine to cool and weigh the flask, the completeness of the 
reaction can be determined. Without weighing, it is very difficult to gauge this reaction as the length 
varies greatly. 

In the summer, in direct midday sunlight, the reaction is complete in a few hours. In winter, or 
low light, the reaction needs 12-24 hours to complete. Adding 4 g of phosphorus pentachloride to 
the toluene can enhance the reaction. The crude benzal chloride thus obtained can be directly used to 
make benzaldehyde. 



benzaldehyde 


c 7 h 6 o 


21 


mp -56.5 


bp 179 


d 1.043 


m 106.12 


c $?.?? 



Safety Data: MSDS 






Jlabguahd* 

: SlQ-iage Coda 








GREEN 









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Megalomania's Precursor Section Part 1 





Synonyms: almond artificial essential oil; artificial almond oil; artificial bitter almond oil; artificial 
essential oil of almond; benzenecarbonal; benzene carboxaldehyde; benzene methylal; benzoic 
aldehyde; benzoyl hydride; oil of bitter almond; phenylmethanal 




Synthesis: To prepare benzaldehvde, start with the crude benzal chloride obtained from its 

synthesis. Into a round-bottomed flask with the benzal chloride, add a solution of 500 mL of wa 
and 150 g of calcium carbonate. Set the flask up for reflux and heat for 4 hours on an oil bath. Keep 
the oil bath at 130 °C by checking the oil itself with a thermometer. 

After refluxing, steam distill the product to obtain crude benzaldehyde oil. (The portion that did 
not distill over contains some benzoic acid. It can be discarded, or purified by filtering while hot 
through a piece of fluted filter paper, then adding concentrated hydrochloric acid to the filtrate. On 
cooling the benzoic acid will precipitate, it is filtered and recrystallized from hot water.) The crude 
benzaldehyde oil is treated with a concentrated solution of sodium bisulfite, after shaking for a long 
time the oil should have dissolved into solution. If any crystals happen to form during the shaking, 
add water until they dissolve. 

After most of the oil is dissolved, filter the solution over fluted filter paper, and then treat the 
filtrate with sodium carbonate until it is strongly alkaline. This liquid is now steam distilled to 
obtain pure benzaldehyde. The product can be further purified by mixing with ether, letting the ether 
evaporate, and distilling (normal, not steam) the benzaldehyde. 

If you have obtained benzaldehyde from other sources, it must be purified if it is anything less 
than ACS grade. It should be washed with sodium carbonate solution, dried, and distilled with 
minimum atmospheric exposure. Only the fraction collected at 178-180 °C is kept. 



benzaldehyde phenylhydrazone 



C 13 H 12 N 2 



22 




mp 158 


bp 327.5 


d? 


m 196.1 


c $?.?? 


Safety Data: MSDS 


ChemAlerl* 
Si-o rage Code 

. GRAY 



Synonyms: benzalphenylhydrazine; benzylidenephenylhydrazine; 
diphenylhydrazone; NSC 37088 




Synthesis: Prepare a solution of 9.81 g of benzaldehyde and 10 g of phenylhydrazine in 100 mL 

of ethyl alcohol. The benzaldehyde should be chilled to 0-5 degrees C before adding it to the 
solution. A cream colored solid should form; allow the solution to stand for 2 hours to complete the 
reaction. The solid is collected by vacuum filtration, washed with ice-cold ethyl alcohol, and dried 
under vacuum. 



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Megalomania's Precursor Section Part 1 



■ 



benzene C 6 H 6 


23 




mp 5.5 bp 80.1 d 0.8787 m 78.11 


; $?.?? 


Safety Data: Flammable, Toxic 


LABGUAiRD* | 
CoEiG 


Synonyms: (6)annulene; benzine; benzol; benzolene; bicarburet of hydrogen; carbon oil; coal 
naphtha; cyclohexatriene; mineral naphtha; motor benzol; nitration benzene; phene; phenyl hydride; 
pyrobenzol 


Synthesis: Nothing yet 



bromine 


X a Y b Z c 


1 


X 

W"7 ? <" 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAlerl 4 
i Siorage CtxJG 




Synonyms: 


Synthesis: Nothing yet 



bromobenzene 


C 6 H 5 Br 


24 


Br 


mp -30.6 bp 156.2 d 1.4952 


m 157.01 


: $?.?? 


Safety Data: Flammable, Irritant 


LABGUARD* I 
Sl.O.'-arjif Coc:e 



Synonyms: monobromobenzene; phenyl bromide 



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Megalomania's Precursor Section Part 1 



Synthesis: To a 250-mL Florence flask connect a vertical tube 50 cm long and 1.5 cm wide, the 

upper end of which is closed by a stopper bearing a narrow glass tube bent at right angles to form a 
U. The other end is connected with a flask containing 250 mL of water , by a stopper having a small 
wedge removed. See the illustration. The tube does not touch the water, but remains about 1 cm 
above the surface. Place 57 mL of benzene and 1 g of iron filings into the first flask. Immerse the 
flask in a salt-ice bath to cool it down. Through the vertical tube add 40 mL of romine , then 
immediately connect the narrow tube. After some time an extremely energetic reaction will begin 
with the evolution of hydrobromic acid gas, which should be completely absorbed by the water. 
Should there be no reaction after a short time, remove the ice bath for a brief period, and if 
necessary momentarily immerse the flask in warm water. As soon as even a weak gas evolution 
begins, the flask is at once cooled again. If you do not cool it right away there is a risk of the 
reaction going out of control, if this happens even with cooling, use larger iron filings or small nails. 

When the reaction has subsided remove the ice bath, dry the flask, and heat until no red bromine 
vapors are visible above the dark colored liquid. The product is shaken with several portions of 
water to wash it, and then steam distilled. As soon as crystals of dibromobenzene (some will always 
form) begin to separate out in the condenser, the receiver is changed and the distillation is continued 
until all of the dibromobenzene has passed over. The liquid portion is added to a seperatory funnel 
where the bromobenzene layer is collected, the water layer is discarded. Add the bromobenzene 
layer to a small Erlenmeyer flask, add a small amount of calcium chloride to dry it, shake the flask 
gently to mix it up. Filter the liquid to remove the calcium chloride, and then add it to a small round- 
bottomed Florence flask. Fractionally distill the liquid to collect pure bromobenzene. The portion 
distilling over between 140-170 °C is collected separately, this portion is fractionally distilled again, 
this time collecting only that which distills over at 150-160 °C. Yield is about 60-70 g. 

The residue boiling above 170 °C remaining the flask after the two distillations contains 
dibromobenzene and hydrobromic acid. These can be disposed of or, since bromine is quite 
valuable, purified and kept. Pour the residue, while still warm, onto a watch glass so it may cool. 
After cooling place the material, along with the other crystals of dibromobenzene, on a porous glass 
plate and press it to separate the acid. Add the pressed dibromobenzene to ethyl alcohol and 
recrystallize, it should now be quite pure. The hydrobromic acid that remains can be purified by 
fractional distillation. The fraction below 126 °C is water, which can be discarded. When the 
temperature reaches 126 and stays constant, begin collecting the distillate; this should be about 48% 
hydrobromic acid. 



calcium carbonate 


CaC0 3 


25 


mp 825 (dec) 


bp- 


d 2.83 


m 100.09 


c $?.?? 





Safety Data: 



UBGUAHD* 
SlQiaye Code 

GREEN 



'O "O' 
C a* 



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Megalomania's Precursor Section Part 1 



Synonyms: aglime; aragonite; atomite; Calcichew; Calcidia; Calcit; calcite; carbonic acid calcium 
salt (1:1); chalk; Citrical; limestone; marble; slaker rejects; vaterite; whiting 

Synthesis: Coming soon! 



calcium chloride 


CaCl 2 


26 


Cl C a — Cl 


mp 772 bp 1600 d 2.152 


m 110.98 


c $?.?? 




Safety Data: Irritant 


LABGUAHD* 
Slorage Code 

GREEN 




Synonyms: calcium dichloride; calcosan; intergravin-orales 



Synthesis: Coming soon! 



calcium hydroxide 



mp - 




d 2.08-2.34 



Safety Data: Corrosive 



Ca(OH 2 ) 
m 74.09 




Synonyms: calcium dihydroxide; calcium hydrate; carboxide; hydrated lime; lime, hydrated; lime 
water; slaked lime 



Synthesis: Coming soon! 



calcium hypophosphite 


Ca(H 2 P0 2 ) 2 


28 






O O 

C 

H H 


mp ? bp ? d ? 


m 170.05 


c $?.?? 


Safety Data: 


j LABGUAflD* 

| Storage Cods 

GREEN 




Synonyms: 



Synthesis: Nothing yet 



http://www.roguesci.org/megalomania/synth/synthesisl.html (21 of 24)12-8-2004 17:24:27 



Megalomania's Precursor Section Part 1 



I 



calcium sulfate 


X a Y b Z c 


1 


X 

W"/ ? N 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAlerl* 
Sic ra ge Code 

GRAY 




Synonyms: 


Synthesis: Nothing yet 



carbanilide 


C 6 H 5 NHCONHC 6 H 5 




mp 238 


bp 260 
(dec) 


d 1.239 


m 212.25 


Safety Data: 




Synonyms: N,N'-diphenylurea\ acardite; N,N'-difenylmocovina; diphenylcarbamide; diphenylurea; 
1,3-diphenylurea; 3-diphenylurea; s-diphenylurea; sym-diphenylurea; karbanilid; N-phenyl-N 1 - 
phenylurea; urea, 1,3 -diphenyl-; USAF ek-534 



Synthesis: Prepare a solution of 390 g of aniline hydrochloride and 190 g of urea in 1500 mL of 

water . Add the solution to a 3-L Florence flask and reflux at its boiling point for 2 hours. After 
reflux, rapidly suction filter the solution to collect the crystals, and then wash the carbanilide with 
100 mL of boiling water. The filtrate is chilled, and the phenylurea that crystallizes out is filtered off 
and rinsed with a little cold water, the washing being discarded. The filtrate is again boiled under 
reflux for 2 hours, or until it begins to bump, and the filtration process is repeated. The filtrate is 
again refluxed and filtered a third time, and each time the phenylurea is collected from the cold 
filtrate. The filtrate is finally evaporated to half of its original volume, and additional crops of 
carbanilide and phenylurea are so obtained. The filtrate can now be discarded. 

The crude carbanilide can be purified be recrystallizing from ethyl alcohol with the use of some 
decolorizing carbon, you will need 1 L of alcohol per 25 g of carbanilide. The yield is about 40%. It 
may be more practical to use only a fraction of the reactants for this lab, say a tenth, and make 
multiple batches. The final purification can be done all at once. 



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Megalomania's Precursor Section Part 1 



All of that phenylurea can be discarded, or kept, I know of no use for it. If you are keeping it, it 
can be purified by dissolving it in the minimum quantity of boiling water, adding a little 
decolorizing carbon, and filtering to remove any impurities. When the filtrate first begins to cool, a 
precipitate of carbanilide is deposited; this must be filtered off while the liquid is still hot. On 
cooling, pure phenylurea will precipitate. The yield here is about 50-55%. 



carbon dioxide 


X a Y b Z c 


1 


X 

W"/ ? N 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAlcrO 
i Siorage Coda 

GflAY 




Synonyms: 


Synthesis: Nothing yet 







carbon disulfide 


cs 2 


30 


S C S 


mp -111.6 


bp 46.5 


d 1.2632 


m 76.14 


2 $?.?? 


Safety Data: Flammable, Toxic 


lasguard* 

Storage Cocje 




Synonyms: alcohol of sulfur; carbon bisulfide; carbon bisulfuret; carbone; carbonio; carbon sulfide; 
dithiocarbonic anhydride; kohlendisulfid; koolstof disulfide; NCI-C04591; Rcra waste number P022; 
schwefelkohlenstoff; solfuro di carbonio; sulfocarbonic anhydride; UN 1131; weeviltox; wegla 
dwusiarczek 


Synthesis: Coming soon! 








carbon tetrachloride 


CC1 4 


31 


Cl 

C,-V CI 

Cl 


mp -23 


bp 76.7 


d 1.589 


m 153.82 


2 $?.?? 


Safety Data: Toxic 


LAfiGUARD' 

: Storage Code 

BLUE 





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Megalomania's Precursor Section Part 1 



Synonyms: tetrachloromethane; Benzinoform; carbona; carbon chloride; carbon tet; flukoids; 
methane tetrachloride; Necatorina; necatorine; perchloromethane; R 10 (refrigerant); refrigerant 
RIO; tetrachlorocarbon; tetrafinol; tetraform; tetrasol; univerm; vermoestricid 

Synthesis: Nothing yet 



NextIPage U Page 2 I Page 3 I Page 4 I Page 5 



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Lab Skills ! Lab Equipment ! Safety ! Roque Science ! Links | What's New | Contact Me | Dj 




Megalomania's Controversial Chem Lab ©1997-2004 /synthesisl/ revised March 15, 2004 



er 



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http://www.roguesci.org/megalomania/safety/acetaldehydemsds.html 



B#e V& “*2a £[j BU-f u° o?AmP YA HA~^)D » A AE?p+ 



"•“•<ueT w— F-a‘£ 4 (E6™Ae M 



http://www.roguesci.org/megalomania/safety/acetaldehydemsds.htmll2-8-2004 17:24:28 




Table Key 



This website uses a verity of abbreviations and key words to describe the physical and chemical 
properties of explosives, chemical weapons, and their precursors. Most of these properties are listed in 
handy informative tables at the top of each substances page. To assist the viewer in better understanding 
these tables this guide has been created. What follows are actual tables taken from the site followed by 
an explanation of what each cell means. 



Explosives Table 





melting point 
91 °C 


boiling point 
explodes 


chemical name 


molecular mass 
222.1 g/mol 


density 
1.18 g/mL 


table key 


sensitivity 
very high 


chemical formula 
C 9 H 18°6 


explosive velocity 
5300 m/s 


estimated cost 

$?.00 /g 



Melting point: the temperature in degrees Celsius at which the explosive melts. 

Boiling point: the temperature in degrees Celsius at which the explosive boils. 

Chemical name: the common name of the explosive. This is usually a non-IUPAC name or acronym. 
Molecular mass: the mass in grams of 1 mole of the explosive. 

Density: the mass in grams of 1 milliliter, or 1 cubic centimeter, of the explosive typically at room 
temperature. Some densities are low average density reflecting that which an improvised chemist is 
likely to obtain, not maximum densities obtainable only by specialized hydraulic equipment. 

Table key: a link to this page. 

Sensitivity: a relative comparison based on TNT of the ease by which this explosive can detonate. 
Primary explosives are very easy to detonate and are therefore considered very sensitive. High 
explosives are generally difficult to detonate and are therefore considered insensitive. This rating is 
purely arbitrary in most cases and should not be considered a definable property of any explosive. 
Chemical formula: the molecular formula of the explosive. Some formulas may be structural and others 
may be ionic, but most are in their condensed form starting with hydrogen, followed by carbon, and then 
all other elements in alphabetical order. 

Explosive velocity: the velocity of detonation given in meters per second based on the given density. 
Some explosive velocities are based on the maximum obtainable density given in the literature, and not 
the listed density. 

Estimated cost: the cost of 1 gram of the explosive using commercially available precursors. These 
costs have not yet been calculated for all explosives. 

Chemical Weapons Table 



| 














melting point 

? °C 


boiling point 

? °C 


chemical name 


molecular mass 
? g/mol 


density 
? g/mL 



http://www.roguesci.org/megalomaniaytablekey.html (1 of 2)12-8-2004 17:24:29 



Table Key 



table key 


toxicity 

? 


chemical formula 
C x H y O z 


ld 50 
x mg/Kg 


estimated cost 

$?.00 /g 



Melting point: the temperature in degrees Celsius at which the chemical melts. 

Boiling point: the temperature in degrees Celsius at which the chemical boils. 

Chemical name: the common name of the chemical. This is usually a non-IUPAC name or acronym. 
Molecular mass: the mass in grams of 1 mole of the chemical. 

Density: the mass in grams of 1 milliliter, or 1 cubic centimeter, of the chemical typically at room 
temperature. 

Table key: a link to this page. 

Toxicity: a relative scale used to designate the lethality of the chemical. This rating is purely arbitrary as 
almost all of the chemicals are deadly, but the extent to which they are is described in the table. 
Chemical formula: the molecular formula of the chemical. Some formulas may be structural and others 
may be ionic, but most are in their condensed form starting with hydrogen, followed by carbon, and then 
all other elements in alphabetical order. 

LD 50 : this data is the lethal dose required to induce death in 50% of all experimental trials. These results 
are usually determined on rats. The given number is the amount of poison, given in milligrams, that 
must be ingested, inhaled, or absorbed for each kilogram of body mass of the victim. The lower this 
number the more lethal the compound. 

Estimated cost: the cost of 1 gram of the chemical using commercially available precursors. These 
costs have not yet been calculated for all chemicals. 

Home | Explosives l Chemical Weapons ! Pharmaceuticals | Pesticides | Precursors 
Lab Skills | Lab Equipment ! Safety j The Forum | Unks | What's New | Contact Me | Disclaimer 



http://www.roguesci.org/megalomaniaytablekey.html (2 of 2)12-8-2004 17:24:29 



Megalomania's Precursor Section Part 5 



Precursors Part 5 



silver iodide 


Agl 


1 




X 

z 1 

unknown 


mp 552 bp ? d 5.67 


m 234.77 


c $?.?? 


Safety Data: 


\ LABGUAHD* 

: Storage Cede 

GREEN 




Synonyms: 


Synthesis: Nothing yet 





A 



silver nitrate 


AgN0 3 


1 


X 

W"/ ? X 

z 1 

unknown 


mp 212 


bp 440 dec 


d 4.35 


m 169.87 


2 $?.?? 


Safety Data: Corrosive 


LARGUARD* 
Storage Code 

WHITE 




Synonyms: 


Synthesis: Coming soon! 




sodium 


Na 


1 


Na 


mp 97.82 


bp 881.4 


d 0.968 


m 22.98977 


2 $?.?? 


Safety Data: Corrosive, Flammable 


Ut&GUAflD* 





Synonyms: natrium 



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Megalomania's Precursor Section Part 5 



Synthesis: Nothing yet 



sodium acetate 


CH 3 COONa 


1 


X 

W'7 ? N, 
z x 

unknown 


mp 58 bp >120 dec d 1.45 


m 82.03 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl* 
Storage Coda 







Synonyms: 



Synthesis: Starting with some acetic acid (in this case a bottle of clear white vinegar, not cider 

vinegar), add enough sodium hydroxide to neutralize the acid. 1 mole of hydroxide will neutralize 1 
mole of acid, so adjust your reactants according to how much you wish to make. It will take about 
126 g of sodium hydroxide to neutralize 4 L of 5% vinegar. It is a good idea to have the solution be 
slightly acidic rather than have excess sodium hydroxide, the acid will be removed later on, the base 
will not. The neutralization will generate a good deal of heat, add the hydroxide slowly with stirring, 
a cooling bath may help. A more economical choice for a neutralizer is sodium bicarbonate, good 
old baking soda. This will be the trite baking soda and vinegar reaction kids love; in this case it will 
take 266.7 g of sodium bicarbonate to neutralize 4 L of 5% vinegar. The level of neutralization can 
be gauged by how much carbon dioxide gas is being released; once the fizzing subsides it is done. 

To obtain the crystals of sodium acetate, boil the neutralized solution down until only crystals 
remain. To obtain anhydrous crystals, place them in a shallow iron, nickel, or ceramic crucible and 
heat with a flame. The salt will first melt from its moisture content, eventually steam will be evolved 
in large amounts and the salt will solidify. To remove the last traces of moisture, heat the mass very 
strongly, wave the flame back and fourth under the crucible until the crystals melt again, it is done. 
Be sure not to overheat the crystals, they will decompose into a flammable gas and begin to char. 
After the crystals have cooled, scrape them from the dish with a knife and seal them, they will 
eventually absorb moisture from the air. If the crystals are kept for any length of time, or if they are 
obtained from a chemical supplier, it is a good idea to melt them to drive off any acquired moisture. 





sodium azide 


NaN 3 


1 




mp dec bp- d 1.846 


m 65.01 


c $?.?? 


Safety Data: Toxic 


LABGUARD' 
Storage Code 

BLU£ 





Synonyms: azide; azium; hydrazoic acid, sodium salt; smite; U-3886 



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Megalomania's Precursor Section Part 5 



Synthesis: Nothing yet 



sodium benzoate 


C 6 H 5 COONa 


1 


X 

w-7 ? x 
Z 1 
unknown 


mp ? bp ? d ? 


m 144.11 


c $?.?? 




Safety Data: MSDS 


jLABGUARD* 

: Sic rage Gods 

green” 




Synonyms: 


Synthesis: Nothing yet 




Synonyms: baking soda; bicarbonate of soda; carbonic acid monosodium salt; carbonic acid sodium 
salt (1:1); col-evac; jusonin; meylon; monosodium carbonate; monosodium hydrogen carbonate; 
NEUT; soda mint; sodium acid carbonate; sodium hydrocarbonate; sodium hydrogen carbonate; 
soludal 





Synthesis: Coming soon! 











sodium bisulfate 


NaHS0 4 


1 








0 


mp 315 bp? d 2.435 


m 120.06 


c $?.?? 




Safety Data: Corrosive 


larguard* 
Storage Code 

WHITE 




Na U o UH 

0 



Synonyms: sodium acid sulfate; sodium hydrogen sulfate; sodium hydrogen sulfate monohydrate; 
sodium pyrosulfate; sulfuric acid, monosodium salt 



http://www.roguesci.org/megalomania/synth/synthesis5.html (3 of 15)12-8-2004 17:24:34 



Megalomania's Precursor Section Part 5 



Synthesis: Nothing yet 



sodium bisulfite 


NaHS0 3 


1 


X 

W"7 ? n 

z 1 

unknown 


mp ? bp ? d 1.48 


m 104.06 


c $?.?? 


Safety Data: MSDS 


LABGUARD' 
Storage Code 

BLUE 




Synonyms: sodium acid sulfite 


Synthesis: Nothing yet 




Synonyms: ASH; calcined soda; carbonic acid disodium salt; disodium carbonate; natron; nevite; 
sal soda; soda; soda ash; Solvay soda; thermonatrite; washing soda 



Synthesis: Nothing yet 



sodium chlorate 


NaC10 3 


1 


0 

w 

Cl cr H 3 + 

// 

0 


mp 248 bp 300 dec d 2.5 


m 106.44 


c $?.?? 


Safety Data: Oxidizer 


Ghenri Alert* 
Storage Code 

YELLOW 




Synonyms: Altacide; chlorate of soda; Chlorax; chloric acid, sodium salt; Defol; Dervan; Drop- 
Leaf; Fall; Harvest- Aid; Shed-A-Leaf 'L'; soda chlorate; Tumbleaf 


Synthesis: Nothing yet 



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Megalomania's Precursor Section Part 5 



sodium chloride 


NaCl 


1 


mp 804 bp? d 2.17 


m 58.44 


c $?.?? 


Safety Data: 


j LABGUAfiD* 

: Sloracje Cede 

( GREEN 







Synonyms: common salt; dendritis; extra fine 200 salt; extra fine 325 salt; halite; h.g. blending; 
NaCl; Purex; rock salt; saline; saline solution; salt; sea salt; stat trak plus; sterling; table salt; top 
flake; white crystal 


Synthesis: You don't need me for this one I hope! 





sodium dichromate Na 2 Cr 2 0 7 


1 


X 

W"/ ? n 

z 1 

unknown 


mp 356.7 bp 400 dec d 2.348 m 261.97 


c $?.?? 


Safety Data: Oxidizer, Toxic 


Chem Alert 1 
Storaga Code 

YELLOW 










Synonyms: bichromate of soda; sodium bichromate 


Synthesis: Nothing yet 



sodium hydroxide NaOH 


1 


Na + OH' 


mp 318 bp? d 2.13 m 40.00 


c $?.?? 




Safety Data: Corrosive 


LABGUARD* 
Storage Code 

WHITE 




Synonyms: Augus Hot Rod; caustic lye; caustic soda; lye; Red Devil Lye; soda lye; sodium 
hydrate; white caustic 


Synthesis: Coming soon! 



http://www.roguesci.org/megalomania/synth/synthesis5.html (5 of 15)12-8-2004 17:24:34 



Megalomania's Precursor Section Part 5 





sodium hypochlorite NaCIO 


1 


X 

^"7 ? V 
z 1 

unknown 


mp 18 bp? d? m 74.44 


c $?.?? 


Safety Data: MSDS 


ChemAlcrP 
. Sio rage Coda 

■GflAY 




Synonyms: bleach; Clorox; Dazzle; Eau de Labarraque 


Synthesis: Sodium hypochlorite is available as ordinary OTC bleach in about 5% concentration 

(Clorox brand for example is 5.25%). While it is possible to use store bought bleach to make 
hydrazine, it may contain undesirable contaminants. The hydrazine lab also specifically requires the 
use of the “normal” hypochlorite solution outlined below. I do not know how much hypochlorite the 
normal solution contains, so I cannot tell you how much bleach to substitute. Some experimentation 
on your part will be in order. 

Prepare a solution of 300 g of sodium hydroxide in 1500 mL of water; add 1500 g of ice to this 
solution. Chlorine gas is then passed into the solution until it has gained 213 g (3 moles) in weight. 
During the chlorine addition the solution must be kept thoroughly cold with ice to prevent the 
formation of chlorates. After all the chlorine has passed in, it is necessary to be certain that the 
mixture is slightly alkaline, since any free chlorine in solution will prevent the formation of 
hydrazine, if that is what this chemical will be used for. 


/ 



A 
















A 







sodium nitrate 


NaN0 3 


1 


0 

Jifk, 

N a + 


mp 308 


bp ? 


d 2.26 


m 84.99 


c $?.?? 


Safety Data: Oxidizer 


Ghem Alerl* 
Silage Code 

YELLOW 





Synonyms: Chile saltpeter; cubic niter; nitrate of soda; nitric acid, sodium salt; soda niter; sodium 
(I) nitrate 

Synthesis: Nothing yet 







sodium nitrite 


NaN0 2 


1 




mp 271 


bp 320 dec 


d 2.17 


m 69.00 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis5.html (6 of 15)12-8-2004 17:24:34 



Megalomania's Precursor Section Part 5 





Safety Data: 4SD Oxidizer, Toxic 


Gharri Alert 1 
Storage Code 

YELLOW 




X 

W"7 ? N 

z 1 

unknown 


Synonyms: erinitrit; nitrous acid sodium salt 


Synthesis: Nothing yet 



sodium sulfate 


Na 2 S0 4 


1 


X 

W"/ ? N 

z 1 

unknown 




mp 800 bp ? d 2.7 


m 142.04 


c $?.?? 




Safety Data: 


jLABGUARD* 

: Sto rage Code 

GREEN 




Synonyms: Glauber's salt; mirabilite; salt cake; thenardite 


Synthesis: Nothing yet 



sodium sulfite 



X a Y b Z c 



1 



mp 



bp ? 



d? 



m 126.04 



c $?.?? 



Safety Data: MSDS 



LABGUAHD* 
Storage Code 



GREEN 






X 

! 

W"/ ? n 



Y 



Z 

unknown 



Synonyms: 

Synthesis: Nothing yet 



starch 


(C 6 Hio0 5 )n 


mp ? 


bp ? 


d? 


m - 



1 

c $?.?? 




http://www.roguesci.org/megalomania/synth/synthesis5.html (7 of 15)12-8-2004 17:24:34 




Megalomania's Precursor Section Part 5 



Safety Data: 



ISPS 



4 






LABGUARD* 
Storage Cede 



GREEN 






X 

! 

W"/ ? x 

z 

unknown 



4 



Synonyms: amylum; Maizena; Mondamin 



Synthesis: Nothing yet 



sulfolane 



C 4 H 8 S0 2 



mp 27.4 



bp 285 



d 1.2606 



m 120.17 



c $?.?? 



Safety Data: MSDS 



ChemAlerl* 
Siorgge Code 






X 

! 

W"/ ? x 



Y 



z 

unknown 



Synonyms: tetrahydrothiophene 1, 1-dioxide 1 , tetrahydrothiophene 1-dioxide; thiophan sulfone 



Synthesis: Nothing yet 



sulfur 



mp 



bp ? 



d 2.06 



m 256.512 



c $?.?? 



Safety Data: 



lAuGuard* I 

Storage Cone 






■■■ 






4 



Synonyms: bensulfoid; Bonide Sulfur Plant Fungicide; brimstone; Clifton Sulfur; Colloidal-S; 
colloidal sulfur; Collokit; Colsul; Corosal D and S; Cosan; COS AN 80; Crystex; Elosal; flowers of 
sulfur; flour sulfur; Golden Dew; Hexasul; Kolofog; Kolospray; Kumulus S; Magnetic 6; Magnetic 
70; Microflotox; precipitated; Security Nutronex; Sefril; Sofril; Sperlox-S; Spersul; Spersul thiovit; 
Sul-Cide; Sulfex; Sulfidal; Sulforon; sulfur atom; sulfur, flowers; Sulkol; Sulsol; Super colloid; 
Super Six; Tesuloid; That F; Thiolux; Thion; THION 80; THION 95; Thiorit; Thiovit; Zolvis 



Synthesis: Nothing yet 






http://www.roguesci.org/megalomania/synth/synthesis5.html (8 of 15)12-8-2004 17:24:34 



Megalomania's Precursor Section Part 5 






sulfur chloride 


S 2 C1 2 


1 


X 

W"7 ? n,, 

z 1 

unknown 


mp -77 bp 138 d 1.6885 


m 135.04 


c $?.?? 


Safety Data: 


ChemAlcn* 

. Siorage Code 

it GRAY 

L— -- — • 




Synonyms: disulfur dichloride; sulfur monochloride; sulfur subchloride 


Synthesis: Nothing yet 



a 



A 



sulfur dichloride 


sci 2 


1 


_ S . 
cr ci 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAlcn* 
i Storage Code 

GflAV 




Synonyms: sulfur chloride 


Synthesis: Nothing yet 



A 



A 




sulfuric acid H 2 S0 4 


1 


HO 


j 

3 OH 


mp3 bp 290 d 1.84 m 98.08 


c $?.?? 


Safety Data: 


LABGUARD* 1 
Storage Code 

WHITE 




3 


Synonyms: Acid Mist; BOU; dipping acid; hydrogen sulfate; oil of vitriol; oleum; sulfur acid; 
sulfuric; vitriol brown oil 


Synthesis: Coming soon! 





A 




tetrafluorohydrazine 


F 4 N 2 


1 




mp ? 


bp ? 


d? 


m? 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis5.html (9 of 15)12-8-2004 17:24:34 



Megalomania's Precursor Section Part 5 



Safety Data: 



— 

ISDS 



4 



« 




LABGUARD* . 

Sto'-iitJb Code 



"N" 

F 



Synonyms: dinitrogen tetrafluoride; hydrazine, tetrafluoro-; N2F4; nitrogen fluoride; 
perfluorohydrazine; UN 1955 



Synthesis: Nothing yet 






toluene 


c 7 h 8 


1 




mp -95 bp 110.6 d 0.866 


m 92.14 


c $?.?? 


i O 



http://www.roguesci.org/megalomania/synth/synthesis5.html (10 of 15)12-8-2004 17:24:35 



Megalomania's Precursor Section Part 5 



Safety Data: Flammable 




Synonyms: methylbenzene ; antisal la; Methacide; methyl-benzene; methylbenzol; monomethyl 
benzene; phenylmethane; phenyl methane; tol; toluol; tolu-sol 

Synthesis: Coming soon! 




trifluoroacetic anhydride 



X a Y b Z c 



mp 7 



bp ? 



d? 



m? 



c $?.?? 



Safety Data: Corrosive 



LABGUARD* 
Storage Code 

WHITE 



X 

V' 

z 1 

unknown 



Synonyms: 





Synthesis: Nothing yet 





trinitro-ra-anisidine 



X a Y b Z c 



mp 7 



bp ? 



d? 



m? 



c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis5.html (11 of 15)12-8-2004 17:24:35 



Megalomania's Precursor Section Part 5 





Safety Data: 


ChemAicrr 
Siorage Code 

GRAY 




^ i 

X 

z 1 

unknown 


Synonyms: 


Synthesis: Nothing yet 



A 



trinitro-m-phenetidine x a Y b z c 


1 


X 

W"/ ? n 
z 1 

unknown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: MSDS 


Chem Alert* 
Storage Code 

G«AY 






Synonyms: 


Synthesis: Nothing yet 



tri s (hydroxy methyl)nitromethane C 4 H 9 N0 5 


1 






mp 180 bp? d? m 151.12 


c $?.?? 




no x 


Safety Data: 


Chem Alert* 
Siorage Code 

GflAY 




0H 



OH 



A 



Synonyms: 2-( hydroxymethyl )-2-nitro- 1,3 -propanediol, Cimcool wafers; hydroxymethyl)-2- 
nitropropanediol; hydroxymethyl)-2-nitropropane-l,3-diol; 2-hydroxymethyl-2-nitropropanediol; 
nitro-2-(hydroxymethyl)- 1,3-propanediol; 2-nitro-2- (hydroxy methyl)- 1,3 -propanediol; 
nitroisobutylglycerine; nitroisobutylglycerol; nitrotris(hydroxymethyl)methane; 
trimethylolnitrome thane; tris-nitro 



http://www.roguesci.org/megalomania/synth/synthesis5.html (12 of 15)12-8-2004 17:24:35 



Megalomania's Precursor Section Part 5 



Synthesis: Add to a 3-necked 1-liter flask, which has been set in a pan of cold water set atop a 

cold hotplate, 150 g of nitromethane and 2 g of potassium carbonate hemihydrate. Gradually add 
200 g of 37% formaldehyde, maintaining the temperature in the flask below 30 °C. Add gradually, 
over a period of 30 minutes, an additional 475 g of 37% formaldehyde, allowing the temperature of 
the mixture to rise to 80 °C. Maintain the solution at 90 °C for 2 hours, connect the flask to a 
vacuum source to evaporate the solution to half of its volume, this will drive off the bulk of the 
formaldehyde. Break the vacuum, dilute with water, and concentrate again under reduced pressure. 
Repeat the dilutations and concentrations until only a faint odor of formaldehyde remains. After 
allowing the mixture to cool, pour the solution over a filter to collect the red colored precipitate. 
Dissolve the crude product in hot alcohol and crystallize by cooling. Recrystallize several times 
from ether. 





trivinyl isocyanurate 


X a Y b Z c 


1 


X 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 




Safety Data: MSDS 


Chem Alcrl* 
Storage Cods 

GRAY 




Synonyms: 


Synthesis: Nothing yet 



urea 


H 2 NCONH 2 


1 






0 


mp 132.7 bp- d 1.32 


m 60.06 


2 $?.?? 


Safety Data: 1SDS 


j LABGUAHD* 

: Storage Cede 

GREEN 





Synonyms: Aquacare/HP; Aquadrate; Basodexan; carbamide; carbamimidic acid; carbonyl 
diamide; carbonyldiamine; Hyanit; isourea; Keratinamin; Nutraplus; Onychomal; Pastaron; 
Ureaphil; Urecare; Urederm; Ureophil; Urepearl 



Synthesis: Coming soon! 



http://www.roguesci.org/megalomania/synth/synthesis5.html (13 of 15)12-8-2004 17:24:35 



Megalomania's Precursor Section Part 5 








zinc 


Zn 


1 


[* 1 



http://www.roguesci.org/megalomania/synth/synthesis5.html (14 of 15)12-8-2004 17:24:35 



Megalomania's Precursor Section Part 5 



mp 419.5 


bp 908 


d 7.14 


m 65.38 


c $?.?? 


Safety Data: Flammable 




LABGUARD* 
Storage Coe e 





X 

! 

W"/ ? n 



Y 



Z 

urjimown 



Synonyms: blue powder 



Synthesis: Zinc is an element so it must be purchased, the kind of zinc needed here is powdered. I 
may yet find a method of preparing powdered zinc, so hang tight. 



A 



name 


X a Y b Z c 


1 


X 

W"/ ? N 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAicn* 
Siqrage Cods 

GSA? 




Synonyms: 


Synthesis: Nothing yet 



Page UPage 2 I Page 3 I Page 4 IPage 5IPrevious 

Home | Explosives ! Chemical Weapons ! Pharmaceuticals ! Pesticides ! Precursors 
Lab Skills ! Lab Equipment ! Safety ! Roque Science ! Unks | What's New | Contact Me | Disclaimer 

Megalomania's Controversial Chem Lab ©1997-2004 /synthesis5/ revised January 31, 2004 



http://www.roguesci.org/megalomania/synth/synthesis5.html (15 of 15)12-8-2004 17:24:35 



Megalomania's Precursor Section Part 3 




Precursors Part 3 




infusorial earth 



No Formula 



mp - 



bp 



d- 



m 



c $?.?? 



Safety Data: 



] labguahB* - 

Storage Cade 

GREEN"' 



X 

W'"/ ? x 

z 1 

unkn#vn 



Synonyms: Celite; diatomaceous earth; fossil flour; kieselguhr; siliceous earth; Super-Cel 
Synthesis: Coming soon! 



A 



iodine 


h 


1 


1 1 


mp 113.60 bp 185.24 d4.93 


m 126.945 


c $?.?? 


Safety Data: Corrosive 


larguard* 
Storage Code 

WHETE 




Synonyms: 


Synthesis: Coming soon! 



iron 


X a Y b Z c 


1 


X 

W"/ ? N 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: SDS 


ChemAlcrl 4 
i Sic rage Code 

GRAY 




Synonyms: 



http://www.roguesci.org/megalomania/synth/synthesis3.html (1 of 17)12-8-2004 17:24:41 





Megalomania's Precursor Section Part 3 





Synthesis: Nothing yet 






isopropyl alcohol CH 3 CHOHCH 3 


1 


OH 


mp -88.5 bp 82.5 d 0.78084 m 60.10 


;$?.?? 


Safety Data: Flammable 


LABGUARD* I 
StO^aoB Cot; e 


Synonyms: 2-propanob, alcojel; alcosolve; alcosolve 2; avantin; chromar; combi-schutz; 
dimethylcarbinol; hartosol; 2-hydroxypropane; imsol a; IPA; i-propanol; isohol; isopropanol; 
lutosol; petrohol; propan-2-ol; n-propan-2-ol; propol; rubbing alcohol; sec-propanol; sec-propyl 
alcohol; spectrar; sterisol hand disinfectant; takineocol 


Synthesis: Coming soon! 


/ 



isopropylamine 


(CH 3 ) 

2 chnh 2 


1 




mp -101 bp 33-34 d 0.694 


m 59.11 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl* 
Sic rage Code 




Synonyms: 2-propanamine; 2-aminopropane; monoisopropylamine; propan-2-amine; sec- 
propylamine 


Synthesis: Nothing yet 



^ ^ ^ ^ — ii 




lead acetate 


Pb 

(CH 3 C00 2 ) 


1 


■vf 'Fb 

0 0 


mp 75 bp 100 dec d 2.55 


m 325.29 


c $?.?? 


Safety Data: Toxic 


] LABGUAHD* 

: Storage Coda 

GREEN 





http://www.roguesci.org/megalomania/synth/synthesis3.html (2 of 17)12-8-2004 17:24:41 




Megalomania's Precursor Section Part 3 



Synonyms: acetic acid, lead(2+) salt; dibasic lead acetate; lead diacetate; lead dibasic acetate; lead 
(II) salt acetic acid; neutral lead acetate; normal lead acetate; salt of Saturn; sugar of lead 

Synthesis: Coming soon! 



lead monoxide 


PbO 


1 






mp 888 bp ? d 9.53 


m 223.20 


c $?.?? 




Safety Data: Toxic 


CliemAlftrl* 
Stooge Code 

YELLOW 






□ 



Synonyms: C.I. 77577; lead ocher; lead oxide; lead (II) oxide; lead oxide (mono); lead oxide 
yellow; lead protoxide; litharge; litharge yellow L-28; massicot; Massicotite; pigment yellow 46; 
plumbous oxide; yellow lead ocher 



Synthesis: Coming soon! 



lead nitrate 


Pb(N0 3 ) 2 




mp ? 


bp ? 


d 4.53 


m 331.21 





Safety Data: 4SDS Oxidizer, Toxic 



1 



c $?.?? 



Gherm Alert* 
Stooge Cocte 



YELLOW 



0 




□ 



Synonyms: lead dinitrate; lead (II) nitrate; nitric acid, lead(2+)salt 
Synthesis: Coming soon! 



magnesium oxide 



mp 2800 bp ? 



d? 



MgO 

m 40.30 



Safety Data: MSDS 



1 



c $?.?? 



| LABGUAHD* 

: Storage Code 

GREEN’ ’ 



Mg^=0 



http://www.roguesci.org/megalomania/synth/synthesis3.html (3 of 17)12-8-2004 17:24:41 



Megalomania's Precursor Section Part 3 





Synonyms: calcined brucite; calcined magnesia; Irtran-5; Magcal; Maglite; magnesia; magnesia 
usta; magnesium monoxide; magnesium oxide, heavy; magnesium oxide, light 




Synthesis: Coming soon! 



magnesium styphnate x a Y b z c 


1 


X 

z 1 

unlmown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: 


ChemAlcrl* 

; Storage Code 




Synonyms: 


Synthesis: Nothing yet 



maltose 



mp 103 



bp ? 



d? 



C 12 H 22°11 



m 342.30 



c $?.?? 



Safety Data: 



is 



| La.BGU.AHD' 
Storage Code 






GREEN 










;.,OH 



OH 



Synonyms: 4-0-alpha-D-glucopyranosyl-D-glucose\ 4-(alpha-D-glucosido)-D-glucose; maltobiose; 
Maltos; alpha-maltose; D-(+)-maltose; malt sugar; Martos-10 



Synthesis: Nothing yet 



mannitol 


c 6 h 14 o 6 


1 


mp 166- bp 290- 
168 295 d 


m 182.17 


c $?.?? 




Safety Data: 


1 labguahd* 

: Storage Cude 


GREEN 




http://www.roguesci.org/megalomania/synth/synthesis3.html (4 of 17)12-8-2004 17:24:41 



Megalomania's Precursor Section Part 3 





Synonyms: cordycepic acid; Diosmol; Manicol; manna sugar; Mannidex; mannite; D-mannitol; 
Osmitrol; Osmosal; Resectisol 


The listed boiling point is at 3.5 mm of Hg Synthesis: Nothing yet 





mercuric nitrate 


Hg(N0 3 ) 2 


1 


6 6 
J K 


3 

Hg ' 3 

W 0 ' 

:i 


mp 79 bp ? d ? 


m 324.60 


c $?.?? 


Safety Data: Toxic 


CbemAlerl* 
Storage Code 

YELLOW 


Synonyms: mercury nitrate; mercury (II) nitrate; mercury pernitrate; nitric acid, mercury salt 


Synthesis: Coming soon! 



mercuric oxide HgO 


1 


Hg 0 


mp 500 dec bp- d 11.14 m 216.59 


c $?.?? 


Safety Data: Toxic 


1 LABGUARD' 

| Storage Code 

BLUE 




Synonyms: mercury oxide; red mercury (II) oxide; Santar; yellow mercury (II) oxide; yellow oxide 
of mercury 


Synthesis: Coming soon! 



mercury 


Hg 


1 


Hg 


mp -38.87 bp 356.72 d 13.534 


m 200.59 


c $?.?? 


Safety Data: Toxic 


LABGUARD' 
Storage Code 

BLUE 





Synonyms: hydrargyrum; liquid silver; Marcero; quick silver; Rathje 



http://www.roguesci.org/megalomania/synth/synthesis3.html (5 of 17)12-8-2004 17:24:41 



Megalomania's Precursor Section Part 3 





Synthesis: Coming soon! 







methenamine C 6 H 12 N 4 


1 


A 

IN — 

[7 T 

N-_ _._-N 


mp 263 dec bp- d? m 140.19 


: $?.?? 


Safety Data: MSDS 


LABGUAfiD* I 
Storage Cot; e 


Synonyms: l,3,5,7-tetmazatricyclo[3.3.1.1 3 ’ 7 ]decane; aceto hmt; Aminoform; Ammoform; 
ammonioformaldehyde; Cystamin; Cystogen; formamine; Formin; HEXA; Hexaform; 
hexamethylenamine; hexamethyleneamine; hexamethylenetetraamine; hexamethylene tetramine; 
hexamethylene triamine; hexamine; hexilmethylenamine; Hiprex; HMT; HMT A; Mandelamine; 
methamin; metheneamine; preparation af; resotropin; 1,3,5,7-tetraazaadamantane; tetraazatricyclo 
[3.3.1. 1(3, 7)]decane; UREX; Uritone; Uroqid; Urotropin 


Synthesis: Nothing yet 





A 



3-methoxy-2,2',4,4',6,6'- 

hexanitrobiphenyl 


X a Y b Z c 


1 


X 

W"/ ? x 

z x 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAlcrO 
Sic rage Code 

GflAY 

- — 




Synonyms: 


Synthesis: Nothing yet 



2-methoxy-2-methyl-4,5- 

imidazolidinedione 


c 5 h 8 n 2 o 3 


1 


mp ? 


bp ? 


d? 


m? 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis3.html (6 of 17)12-8-2004 17:24:41 



Megalomania's Precursor Section Part 3 




ChemAlcrl* 
Siorage Code 



GflAY 



O 

> 

HN 

O 



O 

f 

NH 




\ 



Synonyms: 



Synthesis: This substance is used to prepare the explosive FOX-7. 1 don’t know how long this stuff 
will sit around, so it may be wise to prepare it shortly before its intended use. 

Preparation of 2-methoxy-2-methyl-4,5-imidazolidinedione. Prepare a solution of 69.6 g of 
sodium methoxide in 1100 mL of methyl alcohol in a 2-L round bottomed flask. Add a magnetic stir 
bar to the flask and set it up for stirring. While stirring, add 36.48 g of acetamidine hydrochloride to 
the flask and keep stirring until a well mixed suspension forms. Prepare a second solution of 55.88 g 
of diethyl oxalate in 400 mL of methyl alcohol. Attach an addition funnel to the flask and slowly 
add the diethyl oxalate solution drop by drop over a period of 3 hours. Maintain stirring throughout 
the addition. After the addition is complete remove the addition funnel and set up a cold water bath 
for the flask. Insert a thermometer in the flask and slowly add enough concentrated hydrochloric 
acid to lower the pH of the mixture to 9 while keeping the temperature below 30 °C. Use the cold 
water bath as necessary to lower the temperature. 

At this point a precipitate of sodium chloride should have formed. Pour the contents of the flask 
over a filter to remove this solid. The salt collected on the filter paper can be discarded. Pour the 
liquid filtrate back into the flask and set the flask up for a simple distillation. Very gently heat the 
flask to distill off the methyl alcohol. This alcohol should be fairly pure and can be recycled. In this 
situation the flask is distilled to dryness to remove all alcohol and leave a solid white powder. When 
very little alcohol remains reduce the heat to around 30 degrees until dry. At this point this is a 
mixture of waste sodium chloride, 2-methyl-4,5-imidazoledione and our final product. Heat a beaker 
of 320 mL of methyl alcohol to boiling and add it to the flask with the solid. Allow a few minutes 
for the soluble portions to dissolve and immediately filter the liquid while still hot to remove any 
insoluble impurities. Again this is just salt, which can be discarded and the liquid kept. Redistill this 
liquid until a volume of only 320 mL remains, and then place the liquid in a refrigerator to cool 
overnight. This process will convert the 2-methyl-4,5-imidazoledione to the final product. In the 
morning a white crystalline material should have precipitated in the bottom of the flask. Filter this 
liquid to collect the crystals and allow them to dry. The crystals should be 2-methoxy-2-methyl-4,5- 
imidazolidinedione with a yield around 64% or 35-36 g. 







methyl acrylate 


CH 2 =CHCOOCH 3 


1 




mp -76.5 


bp ? 


d 0.9561 


m 86.09 


c $?.?? 



http://www.roguesci.org/megalomania/synth/synthesis3.html (7 of 17)12-8-2004 17:24:41 



Megalomania's Precursor Section Part 3 



Safety Data: 



§1 




ChemAlerl* 
Sic rage Code 


| 


c 


GRAY 



















Synonyms: 2-propenoic acid methyl ester, acrylic acid methyl ester; curithane 103; 
methoxycarbonylethylene; methyl ester acrylic acid; methyl propenoate; methyl 2-propenoate; 
propenoic acid methyl ester 

Synthesis: Nothing yet 



methyl alcohol CH 3 OH 


1 


OH 

H 


mp -97.8 bp 64.7 d 0.7866 m 32.04 


; $?.?? 


Safety Data: Flammable, Toxic 


LA&GUARD* I 
Storage Core 


Synonyms: carbinol; colonial spirit; Columbian spirits; methanol; methyl hydroxide; methylol; 
monohydroxy methane; pyroxylic spirit; wood; wood alcohol; wood naphtha; wood spirit 


Synthesis: Nothing yet 



methylamine 


CH 3 NH 2 


1 


r 


jh 2 


mp -93.5 


bp -6.3 


d 0.699 


m 31.06 


: $?.?? 












LAUGUASD* ! 




Y'*"h 


Safety Data: Flammable, Irritant 




Storage Core 







Synonyms: aminomethane; carbinamine; methanamine; mercurialin; monomethylamine 



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Megalomania's Precursor Section Part 3 



Synthesis: Prepare a solution of 25 g of dried acetamide and 23 mL of bromine in a 500-mL flask. 

Place the flask into a cold water bath. Gradually add a solution of 40 g of potassium hydroxide in 
350 mL of water to the flask until the brownish red color turns to bright yellow, some hydroxide 
solution may remain unused. This mixture is then added to a 1-L flask containing a solution of 80 g 
of potassium hydroxide in 150 mL of water heated to 70-75 °C. The addition should be done by an 
addition funnel in a continuous stream over the course of 2-3 minutes. The liquid is maintained at 
70-75 °C until it becomes colorless, this will take approximately 15-30 minutes. If at any time the 
temperature rises above 75 °C, the flask must be cooled by immersion for a short time in cold water. 

The methylamine that should have formed is then removed by steam distillation; it is collected in 
a receiver containing a mixture of 52 mL of concentrated hydrochloric acid and 40 mL of water. To 
insure that the methylamine is completely absorbed by the acid, it must be bubbled into the receiver 
straight from the condenser. If you are using a vacuum adapter to direct the flow of liquid into the 
receiver, attach a piece of glass tubing to the tip so it extends to the bottom of the receiver. 
Otherwise, just connect a one-hole stopper to the condenser with an angled piece of glass tube 
extending into the bottom of the receiver. Make sure the tube end in the condenser is near the 
bottom of the stopper, not the middle, so the condensed liquid can drain easier. Periodically test the 
pH of the condensed liquid, when it is no longer basic discontinue the distillation. 

The resulting methylamine hydrochloride is partially evaporated in a porcelain dish heated over a 
flame, then to dryness by heating on a water bath. It is finally heated on a hotplate to 100 °C until it 
is dry and dusty. The crude methylamine thus obtained is contaminated with some ammonium 
chloride salt. Grind the dried substance into a fine powder followed by recrystallization from 100% 
ethyl alcohol. Filter to collect the crystals, and then dry them in a desiccator. 



methylene chloride CH 2 C1 2 


1 


H 

H-V CI 

Cl 


mp -95 bp 39.75 d 1.3255 m 84.93 


c $?.?? 


Safety Data: SDS 


.]labguahd* 

j Storage Cede 

GREEN 


Synonyms: dichloromethane; Aerothene MM; DCM; Freon 30; methane dichloride; methylene 
bichloride; methylene dichloride; narkotil; R 30; Refrigerant 30; solaesthin; solmethine 


Synthesis: Nothing yet 







2-methyl-2-nitro- 1 ,3 -propanediol 


c 4 h 9 no 4 


1 




mp ? 


bp ? 


d? 


m? 


c $?.?? 







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Megalomania's Precursor Section Part 3 




Synonyms: 2-methyl-2-nitropropane-l,3-diol; 2-nitro-2-methyl- 1,3 -propanediol; NMPD 



Synthesis: Nothing yet 




A 



metriol 


X a Y b Z c 


1 


X 

z 1 

unknown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: MSDS 


ChemAlcrl* 
Sic ra ge Code 

■Gfl/W 




Synonyms: 


Synthesis: Nothing yet 




naphthalene 


C 10 H 8 


1 


mp 80.2 bp 217.9 d 1.162 


m 128.17 


c $?.?? 




Safety Data: MSDS 


LABGUARD' 
Storage Cede 


BLUE 



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Megalomania's Precursor Section Part 3 





Synonyms: camphor tar; mighty 150; mighty rdl; mothballs; moth flakes; naphthanin; naphthene; 
tar camphor; white tar 




Synthesis: Coming soon! 



3-nitrazabutylamine x a Y b z c 


1 


X 

W"/ ? \ 

z 1 

unknown 


mp ? bp ? d ? m ? 


c $?.?? 


Safety Data: 


ChemAlcrl* 
Sic rage Code 

GfiAY 

— — - • 






Synonyms: 


Synthesis: Nothing yet 



nitric acid 


hno 3 


1 


o 

■ J 

o ty 

\ 

o 

X 


, oo d 1.4134- 

mp -41.59 bp 83 15129 


m 63.01 


c $?.?? 


Safety Data: Corrosive, Oxidizer 


LABGUARD* 
Storage Code 

WHFTE 




Synonyms: aqua fords; azotic acid; fuming nitric acid; hydrogen nitrate; Nital; nitric acid red 
fuming; nitryl hydroxide; red fuming nitric acid; Rfna; Salpetersaure 



Synthesis: The densities listed are for 70% and 100% acid. A density of up to 1.544 can be reached 
with 12.7% dissolved nitrogen dioxide in fuming nitric acid. Nitric acid forms an azeotrope with 
water at 68%, it this has a bp of 120.5 °C (yes, this bp is higher than either water or the acid boils at 
pure). 



nitric oxide 


NO 


1 


mp - 


bp -151.8 


d- 


m 30.01 


c $?.?? 



■|\|:=:n 



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Megalomania's Precursor Section Part 3 



Safety Data: 


ChemAlerO 
Sic rage Code 






GflAY 





Synonyms: mononitrogen monoxide; nitrogen monoxide; nitrogen oxide; NO 



Synthesis: Nothing yet 




m-nitroaniline 


c 6 h 6 n 2 o 2 


1 


mp 114 bp 306 d 0.9011 


m 138.13 


c $?.?? 


Safety Data: 


ChemAlcn* 
i Sic ra ge Co-de 

GflAY 





ID' 



V. 



Synonyms: 3-nitrobenzenamine\ amarthol fast orange r base; m-aminonitrobenzene; l-amino-3- 
nitrobenzene; azobase mna; C.I. 37030; C.I. azoic diazo component 7; daito orange base r; devol 
orange r; diazo fast orange r; fast orange base r; fast orange m base; fast orange mm base; fast 
orange r base; hiltonil fast orange r base; naphtoelan orange r base; nitranilin; m-nitraniline; m- 
nitroaminobenzene; 3-nitroanaline; 3-nitroaniline; m-nitrophenylamine; orange base irga 1 



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Megalomania's Precursor Section Part 3 



Synthesis: Dissolve 10 g of m-dinitrobenzene in 40 mL of ethyl alcohol in a round-bottomed 250- 

mL Florence flask. Place the flask into a salt-ice bath to cool it down; some dinitrobenzene should 
separate out. The solution is then treated with 9 mL of 27-30% ammonium hydroxide. You must use 
only concentrated ammonium hydroxide, adding extra dilute hydroxide will not work in this case. 
Remove the flask from the ice bath and allow it to warm to room temp before proceeding with the 
next step. 

For the synthesis to be most effective it is necessary to weigh the flask (that includes the contents 
of the flask), the following reaction is complete when the weight of the flask has increased by 6 g. 
Saturate the mixture in the flask by bubbling in hydrogen sulfide gas; stop when it appears no more 
is being absorbed. The saturated mixture is now refluxed for 30 minutes. Allow the flask to cool to 
room temperature, and again saturate the mixture with hydrogen sulfide, followed by refluxing. 
Continue the process of saturating and refluxing until the weight increase of 6 g is achieved. 

Without a scale it will be difficult to judge when to stop, some experimentation will be necessary on 
your Part. 

The mixture is now diluted with water, the resulting precipitate is collected on a filter, washed 
with water, and extracted several times by warming with dilute hydrochloric acid. The acidic 
extractions now contain the nitroaniline, it can be precipitated by neutralizing the liquid with 
ammonium hydroxide. The crystals are collected by filtration, and then recrystallized from water. 
The yield is about 70-80%. 



nitrobenzene 


c 6 h 5 no 2 




mp 6 


bp 210-211 


d 1.205 


m 123.11 





Safety Data: Toxic 




Synonyms: essence of mirbane; essence of myrbane; mirbane oil; nitrobenzol; oil of mirbane; oil of 
myrbane 



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Megalomania's Precursor Section Part 3 





Synthesis: Prepare a mixture of 82 mL of 95-100% sulfuric acid and 71 mL of 70% nitric acid in 

a 500-mL flask. Stir well and allow the mixture to cool to room temperature in a cold water bath. 
Gradually add 57 mL of benzene to the acid with frequent shaking. If the temperature rises above 50- 
60 °C during the benzene addition, stop adding benzene and cool the flask in a cold water bath until 
the temperature has lowered. After all of the benzene has been added, reflux the flask in a water bath 
at 60 °C for 1 hour. The temperature of the water bath should be 60 °C, not the contents of the flask. 
Shake the flask frequently during reflux. 

After heating, allow the flask to cool, two layers should form. Transfer the contents to a 
separatory funnel and drain off the bottom layer of sulfuric and nitric acids; the top layer contains 
the nitrobenzene. The bottom layer can be disposed of. The nitrobenzene is then vigorously shaken 
in the separatory funnel several times with water. After each shaking, allow the layers to separate, 
the nitrobenzene will now be the bottom layer, dispose of the top water layer. After washing, place 
the nitrobenzene in a dry Erlenmeyer flask with some calcium chloride. Heat this flask on a steam 
bath, it will first be milky, then it will go clear, stop when it is clear. The nitrobenzene is now 
purified by simple distillation. Yield is about 60-70 g. 





A 



2-nitro-2-(3',5'-dinitrophenyl)- 

propanediol-1,3 


X a Y b Z c 


1 


X 

z 1 

unpown 


mp ? bp ? d ? 


m? 


c $?.?? 


Safety Data: 


ChemAlcrl* 
Siorage Code 

GflAY 




Synonyms: 


Synthesis: Nothing yet 



A 



nitroethane 


ch 3 ch 2 no 2 


1 


O' 


mp -50 bp 114-115 d 1.041 


m 75.07 


c $?.?? 


Safety Data: 


ChemAlcrl* 
i Storage Code 

GRAY 




Synonyms: nitroetan 


Synthesis: Nothing yet 



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Megalomania's Precursor Section Part 3 



nitrogen 


n 2 


1 


X 

%"/ ? > 
z 1 

unknown 


mp -210.01 bp -195.79 d- 


m 28.0134 


c $?.?? 


Safety Data: 1SDS 


ChemAlcrO 
Siorage Coda 

GRAY 




Synonyms: 


Synthesis: Coming soon! 



A 



nitrogen dioxide N0 2 


1 


■+ 

N-__ 

-rr' 0 


mp -9.3 bp 21.15 d 1.448 m 46.01 


c $?.?? 


Safety Data: 


1 LABGUARD' I 
[Storage Code 

BLUE 


Synonyms: nitrogen oxide; nitrogen peroxide; N02 


Synthesis: This is made accidently or as a waste product, I only listed it here because its so 
dangerous. You should know how to avoid making this, as well as how to deal with it if you do. 





nitromethane 


ch 3 no 2 


1 


cu o' 

"n + 


mp -29 bp 101.2 d 1.1322 


m 61.04 


: $?.?? 


Safety Data: 


LABGUARD* ! 



Synonyms: nitrocarbol; NM 



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Megalomania's Precursor Section Part 3 



Because nitromethane is useful as an explosive ingredient, its availability has dried up on the 



OTC market. One of its biggest uses is as automotive fuel for drag racers, they burn 100% 
anhydrous fuel instead of gasoline, but at $25 a gallon or more it's gonna cost ya. This is the same 
stuff used in the bomb at Oklahoma City, and McVeigh tipped off the feds asking for it at a drag 
race. It is also available as a component in fuel for model cars and airplanes at hobby shops, from 
which it can be distilled. Those fuels can be very expensive, however. Hobby shops usually sell it as 
high as 70% with other contaminants in it; they are also wise to someone asking for "the highest 
concentration of nitromethane" you should know exactly what kind of car you need the fuel for if 
you ask. To avoid the hassles of buying this forbidden fuel, I suggest making it yourself. 

Synthesis: Prepare a mixture of 500 g of chloroacetic acid and 500 g of crushed ice in a large 

beaker. Add to this enough cold 40% sodium hydroxide solution to neutralize the acid and make the 
pH of the solution slightly alkaline, about 360 mL should suffice. Do not allow the temperature to 
rise above 20 °C while adding the hydroxide, failing to do so will cause unwanted sodium glycolate 
to form. Prepare a solution of 365 g of sodium nitrite in 500 mL of water . Add this solution to the 
previous solution in a round bottom 3-L Florence flask. 

Set the flask up for pie distillation with the thermometer dipping into the liquid (yes, in the 
liquid, not at the condenser opening like it usually is). Keep the receiving flask cold with an ice 
water bath. Gently heat the solution until bubbles of carbon dioxide are evolved, this should happen 
at around 80 °C. Remove the heat as the reaction should proceed spontaneously, it should rise to 
around 100 °C while the nitromethane/water azeotrope distills over at 90 °C. If the temperature does 
not rise on its own, gently heat the flask to 85°C until it does. At this temperature the exothermic 
decomposition of the reactants becomes so rapid that continued application of heat might cause 
violent frothing, with significant loss of nitromethane. After the reaction subsides to 95-100°C, 
cautiously heat the flask to 1 10 °C, stop when no more nitromethane distills over. 

This should make about 130 mL of nitromethane with 370 mL of water, they should form 
separate layers. Place the layers into a separatory funnel and allow them to stand for 30 minutes, 
afterwards drain off the lower layer of nitromethane. The water layer is mixed with one fourth its 
weight of salt and distilled to give another 10-12 mL of nitromethane. Add this to the nitromethane 
already distilled. The crude nitromethane is dried over anhydrous calcium chloride in a desiccator 
and redistilled to give 115-125 mL of pure nitromethane. 

Yield is about 38%. The yield can be improved slightly by using 625 g of chloroacetic acid and 
450 mL of 40% sodium hydroxide solution. Another increase in yield can be achieved by adding 
374 g of boric acid after adding the sodium nitrite solution, but before doing any heating. You can 
use a smaller flask and do several distillations if you do not have a 3-L flask, just remember to never 
fill it more than two-thirds of the way. 




ext I Page UPage 2 IPage 3I Page 4 I Page 5 I Previous 




Lab Ski 




Explosives ! Chemical Weapons ! Pharmaceuticals ! Pesticides ! Precursors 



Equipment ! Safety ! Roque Science ! Links | What's New | Contact Me | Disclaimer 




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Material Safety Data Sheet 

Acetamide 



ACC# 00110 

Section 1 - Chemical Product and Company Identification 



MSDS Name: Acetamide 

Catalog Numbers: S70042, S70045, A4 250, A4 500, A4-250, A4-500, A4250, A4500, 
S75020, S75021 

Synonyms: Acetic Acid Amide, Ethanamide, Methanecarboxamide. 

Company Identification: 

Fisher Scientific 
1 Reagent Lane 
Fair Lawn, NJ 07410 

For information, call: 201-796-7100 

Emergency Number: 201-796-7100 

For CHEMTREC assistance, call: 800-424-9300 

For International CHEMTREC assistance, call: 703-527-3887 



Section 2 - Composition, Information on Ingredients 



CAS# 


Chemical Name 


Percent 


EINECS/ ELINCS 


60-35-5 


Acetamide 


100 


200-473-5 



Hazard Symbols: XN 
Risk Phrases: 40 



Section 3 - Hazards Identification 



EMERGENCY OVERVI EW 

Appearance: white. Caution! May cause eye and skin irritation. May cause cancer based 
on animal studies. Potential cancer hazard. May cause liver damage. Hygroscopic. May 
cause respiratory tract irritation. 

Target Organs: Liver. 



Potential Health Effects 
Eye: May cause eye irritation. 

Skin: Causes mild skin irritation. 

Ingestion: Ingestion of large amounts may cause gastrointestinal irritation. May cause 



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liver damage. 

Inhalation: May cause respiratory tract irritation. May cause liver damage. 
Chronic: Possible cancer hazard based on tests with laboratory animals. May cause 
cancer according to animal studies. Chronic exposure may cause liver damage. 



Section 4 - First Aid Measures 



Eyes: Flush eyes with plenty of water for at least 15 minutes, occasionally lifting the 
upper and lower eyelids. Get medical aid. 

Skin: Flush skin with plenty of soap and water for at least 15 minutes while removing 
contaminated clothing and shoes. Get medical aid if irritation develops or persists. Wash 
clothing before reuse. 

I ngestion: Do NOT induce vomiting. If victim is conscious and alert, give 2-4 cupfuls of 
milk or water. Never give anything by mouth to an unconscious person. Get medical aid. 
Inhalation: Remove from exposure to fresh air immediately. If not breathing, give 
artificial respiration. If breathing is difficult, give oxygen. Get medical aid if cough or 
other symptoms appear. Do NOT use mouth-to-mouth resuscitation. 

Notes to Physician: Treat symptomatically and supportively. 



Section 5 - Fire Fighting Measures 



General Information: As in any fire, wear a self-contained breathing apparatus in 
pressure-demand, MSFIA/NIOSFI (approved or equivalent), and full protective gear. 
During a fire, irritating and highly toxic gases may be generated by thermal 
decomposition or combustion. Dusts may be combustible when exposed to heat, flame, 
or oxidizing agents. Dust can be an explosion hazard when exposed to heat or flame. 
Extinguishing Media: For small fires, use dry chemical, carbon dioxide, water spray or 
alcohol-resistant foam. Water or foam may cause frothing. Use water spray to cool fire- 
exposed containers. 



Section 6 - Accidental Release Measures 



General Information: Use proper personal protective equipment as indicated in Section 
8 . 

Spills/ Leaks: Vacuum or sweep up material and place into a suitable disposal container. 
Avoid runoff into storm sewers and ditches which lead to waterways. Avoid generating 
dusty conditions. Provide ventilation. Clean up residual material by washing area with a 2- 
5% solution of soda ash. 



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Section 7 - Handling and Storage 



Handling: Minimize dust generation and accumulation. Avoid contact with skin and eyes. 
Avoid ingestion and inhalation. Use with adequate ventilation. 

Storage: Keep from contact with oxidizing materials. Store in a cool, dry, well-ventilated 
area away from incompatible substances. 



Section 8 - Exposure Controls, Personal Protection 



Engineering Controls: Facilities storing or utilizing this material should be equipped 
with an eyewash facility and a safety shower. Use process enclosure, local exhaust 
ventilation, or other engineering controls to control airborne levels. 

Exposure Limits 



Chemical Name 


ACGIH 


NIOSH 


OSHA - Final PELs 


Acetamide 


none listed 


none listed 


none listed 



OSHA Vacated PELs: Acetamide: No OSHA Vacated PELs are listed for this chemical. 

Personal Protective Equipment 

Eyes: Wear appropriate protective eyeglasses or chemical safety goggles as described by 
OSHA's eye and face protection regulations in 29 CFR 1910.133 or European Standard 
EN166. 

Skin: Wear appropriate gloves to prevent skin exposure. 

Clothing: Wear appropriate protective clothing to minimize contact with skin. 
Respirators: Follow the OSFIA respirator regulations found in 29CFR 1910.134 or 
European Standard EN 149. Always use a NIOSFI or European Standard EN 149 approved 
respirator when necessary. 



Section 9 - Physical and Chemical Properties 



Physical State: Solid 
Appearance: white 
Odor: mousy like odor 
pH: Not available. 

Vapor Pressure: Negligible. 

Vapor Density: ~2 
Evaporation Rate:Negligible. 
Viscosity: Not available. 

Boiling Point: 221 deg C 
Freezing / Melting Point:80 deg C 



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Autoignition Temperature: Not applicable. 

Flash Point: Not applicable. 

Decomposition Temperature:Not available. 

NFPA Rating: (estimated) Health: 1; Flammability: 1; Reactivity: 0 

Explosion Limits, Lower:Not available. 

Upper: Not available. 

Solubility: 200% in water. 

Specific Gravity/ Density: 1.16 
Molecular Formula:C2H5NO 
Molecular Weight:59.07 



Section 10 - Stability and Reactivity 



Chemical Stability: Stable at room temperature in closed containers under normal 
storage and handling conditions. 

Conditions to Avoid: Dust generation, moisture, excess heat. 

Incompatibilities with Other Materials: Strong oxidizers, metals, halogenated 
materials. 

Hazardous Decomposition Products: Carbon monoxide, oxides of nitrogen, irritating 
and toxic fumes and gases, carbon dioxide. 

Hazardous Polymerization: Has not been reported. 



Section 11 - Toxicological Information 



RTECS#: 

CAS# 60-35-5: AB4025000 

LD50/ LC50: 

CAS# 60-35-5: 

Oral, mouse: LD50 = 12900 mg/kg; 

Oral, rat: LD50 = 7 gm/kg; 

Carcinogenicity: 

CAS# 60-35-5: 

California: carcinogen; initial date 1/1/90 
OSHA: Possible Select carcinogen 
I ARC: Group 2B carcinogen 

Epidemiology: IARC Group 2B: Proven animal carcinogenic substance of pote ntial 
relevance to humans. 

Teratogenicity: No information available. 

Reproductive Effects: No information available. 

Neurotoxicity: No information available. 

Mutagenicity: No information available. 

Other Studies: See actual entry in RTECS for complete information. 



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Section 12 - Ecological Information 



Ecotoxicity: No data available. No information available. 

Environmental: Terrestrial: Very high leachability due to its solubility. Aquatic: Readily 
biodegrades. Atmospheric: Exists as an aerosol and is removed by wet deposition. Not 
expected to bioconcentrate. 

Physical: No information available. 

Other: For more information, see "HANDBOOK OF ENVIRONMENTAL FATE AND 
EXPOSURE DATA." 



Section 13 - Disposal Considerations 



Chemical waste generators must determine whether a discarded chemical is classified as 
a hazardous waste. US EPA guidelines for the classification determination are listed in 40 
CFR Parts 261.3. Additionally, waste generators must consult state and local hazardous 
waste regulations to ensure complete and accurate classification. 

RCRA P-Series: None listed. 

RCRA U-Series: None listed. 



Section 14 - Transport Information 





US DOT 


1 AT A | RID/ ADR | 1 MO 


Canada TDG 


Shipping 

Name: 


No 

information 

available. 




No information 
available. 


Hazard Class: 








UN Number: 




Packing Group: 



Section 15 - Regulatory Information 



US FEDERAL 
TSCA 

CAS# 60-35-5 is listed on the TSCA inventory. 

Health & Safety Reporting List 

None of the chemicals are on the Health & Safety Reporting List. 

Chemical Test Rules 



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None of the chemicals in this product are under a Chemical Test Rule. 

Section 12b 

None of the chemicals are listed under TSCA Section 12b. 

TSCA Significant New Use Rule 

None of the chemicals in this material have a SNUR under TSCA. 

SARA 

Section 302 (RQ) 

CAS# 60-35-5: final RQ = 100 pounds (45.4 kg) 

Section 302 (TPQ) 

None of the chemicals in this product have a TPQ. 

SARA Codes 

CAS # 60-35-5: chronic. 

Section 313 

This material contains Acetamide (CAS# 60-35-5, 100%), which is subject to the 
reporting requirements of Section 313 of SARA Title 1 1 1 and 40 CFR Part 373. 

Clean Air Act: 

CAS# 60-35-5 is listed as a hazardous air pollutant (HAP). This material does not contain 
any Class 1 Ozone depletors. This material does not contain any Class 2 Ozone depletors. 

Clean Water Act: 

None of the chemicals in this product are listed as Hazardous Substances under the CWA. 

None of the chemicals in this product are listed as Priority Pollutants under the CWA. 

None of the chemicals in this product are listed as Toxic Pollutants under the CWA. 

OSHA: 

None of the chemicals in this product are considered highly hazardous by OSHA. 

STATE 

CAS# 60-35-5 can be found on the following state right to know lists: California, New 
Jersey, Pennsylvania, Minnesota, Massachusetts. 

The following statement(s) is(are) made in order to comply with the California 
Safe Drinking Water Act: WARNING: This product contains Acetamide, a chemical 
known to the state of California to cause cancer. California No Significant Risk Level: 
CAS# 60-35-5: no significant risk level = 10 ug/day European/ International 
Regulations 

European Labeling in Accordance with EC Directives 
Hazard Symbols: 

XN 

Risk Phrases: 

R 40 Possible risks of irreversible effects. 

Safety Phrases: 

S 36/37 Wear suitable protective clothing and 
gloves. 

WGK (Water Danger/ Protection) 

CAS# 60-35-5: 1 

Canada 

CAS# 60-35-5 is listed on Canada's DSL List. CAS# 60-35-5 is listed on Canada's DSL 



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List. 

This product has a WHMIS classification of D2A. 

CAS# 60-35-5 is not listed on Canada's Ingredient Disclosure List. 

Exposure Limits 

CAS# 60-35-5: OEL-FI NLAND; Carcinogen OEL-GERMANY; Carcinogen 



Section 16 - Additional Information 



MSDS Creation Date: 12/16/1998 
Revision #6 Date: 3/16/2001 

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Megalomania's Method of Making Acetone Peroxide 




melting point 
91 °C 


boiling point 
explodes 


acetone peroxide 


molecular mass 
222.1 g/mol 


density 
1.18 g/mL 


table kev 


sensitivity 
very high 


chemical formula 
C 9 Hi 8 0 6 


explosive velocity 
5300 m/s 


estimated cost 
$7.00 /g 



ch 3 

H3C-C- 0 - 

0 

1 

o 

H3C-C-0" 

CH? 



o ch 3 
c 

o ch 3 



Narrowing down a name for this compound is rather tricky. In the literature is is commonly referred to as 
acetone peroxide because it is typically a mixture of isomers. Other literature refers to it as 
tricycloacetoneperoxide, triacetonetriperoxide, TATP, AP, TCAP, and 3,3,6,6,9,9-hexamethyl- 1 ,2, 4, 5, 7, 8- 
hexoxonane. Many types of chemicals react with air and light to form explosive peroxides, usually this is a bad 
thing because their formation occurs without intent. A compound being distilled in the lab may explode if 
peroxides have formed, this is why a small amount of liquid is always left undistilled. 

This particular formula is intriguing because of its simplicity to make and the availability of the chemicals used. 
This simplicity has made it very popular among fools. Instruction derived from the Big Book of Mischief, and their 
loathsome breed, are lacking in detailed information that may determine a continued success or failure at this 
procedure. An abundance of misinformation has led to much confusion about acetone peroxide. The information 
presented here is directly from the original scientific references by the scientists who developed this explosive, not 
some "crap book" as listed above. There are actually two isomers of acetone peroxide, the first is tricycloacetone 
peroxide, which is what will be made here, and the second is dicycloacetone peroxide. Both of these compounds 
are very similar, but the reaction seems to favor the tricyclo over the dicyclo at lower temperatures. The tricyclo 
isomer is more stable and more powerful than the dicyclo, that is why every effort is made to prepare the former. 
Both isomers will be made in the reaction with the tricyclo being the principal product. There are also a varity of 
other peroxides made in this synthesis; see the reaction scheme below. 

Acetone peroxide would have made a decent military explosive if not for its instability. It can not be stressed 
enough how unstable and dangerous acetone peroxide is. As instability goes this is among the most unstable of 
other explosives here. 

Acetone peroxide is formed by acid-catalyzed nucleophilic addition. That means an acid helps the peroxide, a 
nucleophile, react with the acetone, a ketone. A nucleophile is a "nucleus lover," or a chemical species that donates 
electrons. A ketone is a substance that has the molecular formula R 2 C=0 where R is any carbon chain. There is 



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Megalomania's Method of Making Acetone Peroxide 



some confusion as to which acid to use, the useless internet books frequently cite hydrochloric acid as the acid to 
use. The fact is, the acid is only a catalyst, it does not matter what acid is used, as long as it is a strong acid. Only 
inorganic acids fit this criteria. Since the original literature uses sulfuric acid, this lab uses sulfuric. You may use 
whichever acid is the most economical, or available. 

Acetone, hydrogen peroxide, and sulfuric acid, the chemicals used in this lab, are all available over the counter. 
That is the real reason this explosive is so popular, it is unfortunate that this explosive is so dangerous. Since 30% 
hydrogen peroxide is hard to obtain, substituting 10 times the volume of commercially available 3% peroxide is 
acceptable, although this will lower the yield a bit. It is also advisable to multiply the volume of acid by a 
corresponding value. 






Ketone 


peroxide reaction scheme: 




OH 


hThjO, ? 


U 1 


Uxl 












O 1 


OH 




OH 




OH 

1 


OOH RjC - 


0 


— ► 


o- 

1 


0 

1 

O 


i 

-CRo 






OOH OH 
I 

P' h C — O — O — ( 



OOH OOH 



Rot 1 — ■ O ... 



r i 



o. 

R2C-0" 



o 



p,. hLhjOj^. 


R -i A — < i — f i 


— r 


.p hLhjOj \ / 




jU 




- ,, TI o-o 

OOH 

1 








R.jC — 0 — 0 — CRj — O - 0 — 


0 

1 


OH 




OOH 

1 


-2 + RjC 


-fo-o-c 


r-7 


1 

-0—0— CRo 




1 




n 



DOH 





CHEMICALS 


APPARATUS 






acetone 


500-mL beaker 






ethyl ether 


eye dropper 






hydrogen peroxide 


graduated cylinder 






sulfuric acid 


separatory funnel 


distilled water 


stirring rod/stirrer 



thermometer 



To a 500-mL beaker add 50 mL of acetone , then stir in 30 mL of 30% hydrogen peroxide . Place the beaker in a 
salt-ice bath and cool it to 5° C. After cooling, slowly add 3 mL of 75% sulfuric acid drop by drop with an eye 
dropp . Stir the mixture continuously while adding the acid, keep the temperature between 5° C to 10° C, stop 



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Megalomania's Method of Making Acetone Peroxide 

adding acid if the temperature gets to high. It is very important that you moderate the reaction, high temperatures 
will lower your yield and cause the formation of the less useful dicyclo isomer. After adding all the acid, continue 
stirring for 5 minutes. Keep the mixture in the bath for 1 to 3 hours, or even up to 24 hours. After sitting, a white 
precipitate should have formed. Filter the mixture to collect the crystals, then wash them with 300-500 mL of 
water . Allow the crystals to dry before using, keep them damp if storing. For increased purity, add the precipitate 
to ethyl ethe and let it dissolve. Place the ethyl ether solution in a separatory funnel and wash by shaking with 
three portions of cold water. Add the ethyl ether solution to a beaker and heat it on a steam bath to evaporate the 
ethyl ether. It should take about 3 hours to dry. You will need a graduated cylindei for measuring liquids, a stirring 
rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature. 

I would suggest making this explosive shortly before it is desired to use it as it is never wise to keep unstable 
primary explosives around too long. It can be stored rather safely under water for some time. If allowed to stand in 
the open it will vaporize after some weeks. If stored in a sealed container it may crystallize into the crevaces of the 
cap which could detonate from the friction of opening. Mixing with RDX, PETN, or picric acid will improve the 
stability of this explosive. 




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Comprehensive Organic Chemistry Vol. 1 



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Megalomania's Method of Making Allyl Hydroperoxide 




A 



melting point 
explodes 


boiling point 


allyl hydroperoxide 


molecular mass 
74.10 g/mol 


density 
? g/mL 


table key 


sensitivity 
very high 


chemical formula 
CH 2 =CHCH 2 OOH 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





^ — O-OH 


<s> 







Allyl hydroperoxide can also be called 2-propenyl hydroperoxide. This extremely unstable compound 
must be kept away from all forms of heat and friction. A small amount of rather excessive precautions, 
namely a red light are quite necessary. This compound is stable under UV light but normal light can be 
hazardous. Like all explosive peroxides, this one does not want to exist for long. I would suggest 
keeping it refrigerated and in the dark to avoid an untimely detonation. 





CHEMICALS 


APPARATUS 




allyl methanesulfonate 


beaker 


ethyl ether 


Erlenmeyer flask 


hydrogen peroxide 


graduated cylinder 




methyl alcohol 


pipet/buret 




potassium hydroxide 


thermometer 






water 



Prepare a solution of 10.8 g of allyl methanesulfonate and 40 mL of 30% hydrogen peroxide 
dissolved in 30 mL of methyl alcoho in a small >eaker . Prepare a second solution of 10.1 g of lotassium 
hydroxide dissolved in 10.1 mL of water , cool this solution to 0 °C and keep it in a salt-ice bath. With 
extreme caution, add the allyl methanesulfonate solution by dropwise addition to an Erlenmeyer flask 



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Megalomania's Method of Making Allyl Hydroperoxide 



containing the potassium hydroxide solution in the salt-ice bath using a dropper pipet or a buret . The 
addition must be completed in a room illuminated with one of those darkroom red lights as other light 
will cause the allyl hydroperoxide to explode, a safer bet would be to cover all glassware with aluminum 
foil to keep out all light. The product is purified by vacuum distillation followed by extraction with ethyl 
ether . It can be further purified by liquid chromatography. The yield is quite low, 58 mg after 
chromatographic distillation. You will need a graduated cylinder to measure liquids and a thermometer 
to check the temperature. 




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Journal of the American Chemical Society 



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Megalomania's Method of Making Ammonium Nitrate 






melting point 
169.6 °C 


boiling point 
210 °C 


ammonium nitrate 


molecular mass 
80.043 g/mol 


density 
1.725 g/mL 




table kev 


sensitivity 
very low 


chemical formula 
NH 4 NO 3 


explosive velocity 
? m/s 


estimated cost 

$?. 00 /g 


A 









H 






x: 






Ammonium nitrate is used as a fertilizer and is supposed to be available from agricultural supply 
stores or perhaps well stocked garden shops. It may be increasingly hard to find due to its ease of use as 
an explosive, and especially from the Oklahoma City bombing. The government wants to make it less 
dangerous by coating the fertilizer pellets with a special chemical. It took me five minutes of research to 
devise a way of thwarting that method. The proposed anti-explosive would use a similar compound, I 
think it is ammonium sulfate, mixed in with the ammonium nitrate. Ammonium nitrate is very 
hygroscopic, or water absorbing, so it completely dissolves in water, but the new stuff is only partially 
soluble in water. It should not be too difficult to crush up all the nitrate/sulfate nitrate mix, dissolve it in 
water, and skim off what does not dissolve after a few minutes. Of course it's not all that difficult to 
make your own. Ammonium hydroxide, the main ingredient, can be obtained in dilute solution as a 
laundry substance or as a window cleaner, it is ammonia. It is important to get a brand that does not have 
any fragrance, color, or soap additives in it as it may affect the reaction. More information about 
ammonium hydroxide is in the chemical synthesis section. The other chemical is nitric acid, that will be 
far more difficult to obtain and far to precious for most people to make simple ammonium nitrate with. 





CHEMICALS 


APPARATUS 


ammonium hvdroxide 


beaker 


nitric acid 


500-mL Erlenmever flask 



water 



litmus paper 



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Megalomania's Method of Making Ammonium Nitrate 



The ammonium nitrate is formed by a simple double displacement reaction when the ammonium ion, 
NH 4 +, replaces the H+ ion from the nitric acid and bonds to the remaining nitrate ion, N0 3 , then the H+ 
ion forms water from the hydroxide ion, OH-, left by the ammonium ion. The equation is NH 4 OH + 
HN0 3 = NH 4 NO 3 + H 2 0 

Into a 500-mL Erlenmeyer flask , add 100 mL of water then add 100 mL of concentrated nitric acid . 
Always add acid to water, not the reverse, because the acid will splash when water is added. Slowly add 
ammonium hydroxide from a beaker to the Erlenmeyer flask while stirring by swirling the flask 
occasionally until the mixture is alkaline to litmus paper . Keep the flask in a salt-ice bath to keep it cool, 
and add the ammonium hydroxide in small portions so it may cool a bit. If the reaction gets too hot it 
will instantly come to a boil and splatter acid all over the place (the first time that happened to me I 
dropped the whole damned beaker of ammonium hydroxide when I jumped back quite startled, the 
second time I lost most of my product when it splattered out of the flask). Remember that red litmus 
turns blue in the presence of base and blue turns red in the presence of acid. Gently boil the mixture until 
only a crust remains. Let the remaining water evaporate or heat gently to drive out the remaining 
moisture, you can use an oven for this. Ammonium nitrate will draw moisture from the air so keep it 
tightly sealed right after you are done heating it. If strongly heated the ammonium nitrate will 
decompose to form litrous oxide , which is laughing gas, and then will begin to emit white fumes. If you 
see white fumes stop heating because that's one step from detonation, don't get too worried though the 
detonation temperature is several hundred degrees above the fumes stage. 

It seems wasteful to use all that nitric acid just to make this particular substance, but knowledge is 
power! I have never actually seen ammonium nitrate for sale in an agricultural supply store, I have also 
never been in an agricultural supply store, so that may be why. This chemical is so insensitive to 
detonation that you could store it under your bed and have more worries about your pillow blowing up 
than the ammonium nitrate. When mixed with a sensitizer like diesel oil, kerosene, gasoline, 
nitromethane, hydrazine and the like it becomes quite sensitive. 






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Megalomania's Method of Making Ammonium Nitrate 




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Megalomania's Method of Making Ammonium Picrate 




A 




melting point 
265-271 °C 


boiling point 
decomposes >265 °C 


ammonium picrate 


molecular mass 
246.14 g/mol 


density 
1.60 g/mL 


table key 


sensitivity 
very low 


chemical formula 
C 6 H 2 (N0 2 ) 3 0NH 4 


explosive velocity 
7040 m/s 


estimated cost 

$?.00/g 





A 




Ammonium picrate, also called 2,4,6-trinitrophenol ammonium salt, ammonium trinitrophenolate, 
Dunnite, or Explosive D, is prepared in much the same way as nitrogen triiodide. Ammonium picrate 
was first prepared in 1841 by a scientist named Marchand. It was not used until 1869 when it was mixed 
with potassium nitrate as a propellent for rifles. Alfred Nobel patented it in 1888 for Dynamites. The US 
Army picked it up in 1901, and the Navy floated it in 1907. It saw peak production during WWII but has 
since fallen victim to progress in chemistry. This explosive is relatively stable, therefore safer to prepare 
and handle. The only real problem is getting ahold of picric acid which is a regulated explosive 
chemical. Very few laboratories still use life threatening carcinogens like benzene or explosives like 
picric acid. That means even if you have the authorization to purchase chemicals you will have a hard 
time getting any. Not to worry, I have included the preparation of picric acid. Benzene is another matter 
unfortunately. 





CHEMICALS 


APPARATUS 




ammonium hydroxide 


250-mL beaker 




picric acid 


graduated cylinder 



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Megalomania's Method of Making Ammonium Picrate 



hotplate 



2,4,6-Trinitrophenol ammonium salt is formed when the ammonium ion, NH 4 + , attaches itself to the 

phenol group, OH, of picric acid. I suppose the H from OH is stripped away making O' that balances the 
positive ammonium ion. To make, dissolve picric acid in excess ammonium hydroxide. Add 1 g of 
picric acid to a 250-mL beaker then add 100 mL of hot concentrated ammonium hydroxide . Once the 
picric acid has dissolved, some will precipitate out of solution upon cooling. The liquid must be 
evaporated to fully precipitate the crystals. Evaporation can be accelerated by heating the solution on a 
hotplate or in a heated pan of water. More ammonium picrate can be prepared at once by using the same 
1: 100 ratio of grams picric acid to milliliters ammonium hydroxide. You will need a graduated cylinder 
to measure the liquid. 

The pure substance occurs in two forms, a stable form which is bright yellow and a less stable form 
which is bright red. The crystals which separate here are the red form. The yellow form can be procured 
by recrystallizing the red several times from water. The red form will eventually change into the yellow 
form if stored as a concentrated solution. Keep this material as dry as possible. 




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Megalomania's Method of Making Picric Acid 






melting point 
122 °C 


boiling point 
explodes over 300 °C 


Picric Acid 


molecular mass 
229.11 g/mol 


density 
1.763 g/mL 


table key 


sensitivity 

medium 


chemical formula 

c 6 h 3 n 3 o 7 


explosive velocity 
7480 m/s 


estimated cost 

$?.00/g 






Picric acid, or 2,4,6-trinitrophenol, has also been called picronitric acid; carbazotic acid; nitroxanthic 
acid; melinite; lyddite; pertite; shimose; melinit; granatfullung; sprengkorper 88; pertit; picrinit; ekrasit; 
TNF; and shimoza. Picric acid is both a useful explosive compound and a precursor to other explosives. 
It does not see much use now a days as a laboratory reagent or explosive. It is too dangerous for the lab 
and too costly for the battlefield. I found a very old bottle in the lab once, the bottle had not been used 
for 5 years and should not have been there. It is stable unless old, it will form a very unstable crystalline 
structure after many years. I have three different methods of synthesizing picric acid. The first is a 
laboratory procedure using fairly common chemical reagents, it will provide a better and cheaper 
product. The second is a lesser used, but economical, catalytic process for possible large scale 
manufacture, its chemicals are more difficult to get. The third is one of those improvisational procedures 
using aspirin tablets, it sounds feasible. Picric acid was first mentioned in the alchemical writings of 
Glauber in 1742. The old timers made it from nitrating animal horn, silk, indigo, natural resin, and the 
like. Its synthesis from phenol, and the correct determination of its formula, was in 1841. It was not until 
1830 did anybody think to use picric acid as an explosive. Before then it was assumed that only the salts 
of picric acid were explosive, not the acid itself. In 1873 H. Sprengel proved it could be detonated and 
by 1894 the Russians had worked out a method of manufacture for artillery shells. Soon after, every 
military power used picric acid as their primary high explosive material. The 20th century saw the 
decline of picric acid, the replacement being TNT. The downfall was partially due to the acidic nature 
and the sensitivity of picric acid. Today picric acid is more suited to detonators or booster charges. 



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Megalomania's Method of Making Picric Acid 





CHEMICALS 


APPARATUS 


aspirin 


1000-mL beaker 




benzene 


500-mL Erlenmever flask 


ethyl alcohol 


100-mL Florence flask 




mercuric nitrate 


2-L Florence flask 


nitric acid 


glass filter paper 




phenol 


graduated cylinder 




potassium nitrate 


pipet/buret 




sodium nitrate 


stirrer/stirring rod 




sulfuric acid 


thermometer 






water 



Add 24 mL of phenol and 14 mL of 98-100% sulfuric acid to a round-bottomed 100-mL Florence 
flasl and reflux for 6 hours at 120°C on an oil bath. After the material has cooled, it is diluted with 46 
mL of 72% sulfuric acid. Pour the solution from the round bottomed flask into a 500-mL Erlenmeyer 
flask . 175 mL of 70% nitric acid is added dropwise, with a pipet or buret , add the acid very slowly, a 
drop at a time. The addition of nitric acid will cause a vigorous reaction and release toxic gas, use a 
fume hood or go outside. When all of the acid has been added and the reaction has subsided, the mixture 
is heated for 2 hours on a steam bath to complete the nitration. After 8 to 12 hours the picric acid 
crystals should have separated. These crystals will need to be filtered with lass filter paper because of 
the solutions high acidity. Otherwise, pour off most of the acid, dilute with water , and filter with regular 
filter paper. Wash the crystals with several small portions of water and allow to dry in the open air. To 
purify, dissolve the picric acid in 1 L of boiling water per 15 g of crystals, filter while hot and allow to 
cool slowly. Any heavy droplets of brown oil which dissolve slowly during this boiling should be 
discarded. You will need a graduated cylinder for measuring liquids, and a thermometer to monitor the 
temperature. 

This catalytic process skips the roundabout way above and converts benzene directly into picric acid 
in one step. The reagents of this reaction may be a bit hard to come by, however. Prepare a solution of 
10 g of mercuric nitrate in 600 mL of 70% nitric acid. Add this solution to a round-bottomed 2-L 
Florence flask with 228 mL of benzene . Reflux the mixture for 7 hours on a sand bath. Transfer the 
contents of the flask to another flask and listil it with a steam bath (not steam distillation, simple or 
fractional will suffice). Benzene will distill over first, then nitrobenzene, and finally a mixture of 



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Megalomania's Method of Making Picric Acid 



dinitrobenzene and dinitrophenol will come over slowly. The distillation is continued until these volatile 
organics are removed. The remaining residue is filtered while hot to remove any impurities and allowed 
to crystallize, the picric acid that should have crystallized can be purified by recrystallizing from hot 
water. 

This procedure uses aspirin tablets instead of phenol. Crush 100 ispirin tablets to a fine powder. Put 
500 mL of 95% ethyl alcohol in a 000- mL beaker then add the aspirin powder. Gently heat the alcohol 
while stirring to dissolve the acetylsalicylic acid within the tablets for 15 minutes. Acetylsalicylic acid is 
the active ingredient in aspirin and a phenol derivative. Filter the still hot alcohol to remove any excess 
tablet filler. Now heat the solution to evaporate off all of the alcohol, leaving behind crystals of 
acetylsalicylic acid. When the crystals have dried, add them to a 1000-mL beaker with 700 mL of 95- 
100% sulfuric acid. Heat the acid and stir to dissolve the acetylsalicylic crystals. When all of the crystals 
have been dissolved, add 90 g of sodium nitrate or potassium nitrate . Add a few grams at a time then 
wait for the reaction to subside before adding more. The nitrate addition must be done in a well 
ventilated area as it produces deadly nitrogen dioxide gas. When all of the nitrate has been added, allow 
the mix to cool to room temperature, stirring it every few minutes. Pour it into 1500 mL of ice water to 
precipitate the picric acid. Decant about 1000 mL of the acid water mix then add another 1000 mL of 
water. Filter the solution to collect the picric acid crystals. You may purify the crystals as per method 
one. You will need a stirring rod or magnetic stirrer for mixing. 




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Megalomania's Method of Making <i>m</i>-Picrylpicryl Chloride 




m-Picrylpicryl Chloride 








melting point 
186 °C 


boiling point 

? °C 


m-picrylpicryl chloride 


molecular mass 
458.72 g/mol 


density 
? g/mL 


table key 


sensitivity 

? 


chemical formula 
(0 2 N) 3 (C1)C 6 HC 6 H 2 (N0 2 ) 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 






ra-Picrylpicryl chloride has also been called 3-chloro-2,2',4,4',6,6'-hexanitrobiphenyl, and PIPIC1. It 
has the appearance of pale yellow crystals and was first developed by J.C. Dacons & M.J. Kamlet round 
abouts 1966. As for useful information, other than the fact it is explosive, I have no more. 



CHEMICALS 



benzene 



n-hexane 



3-methoxy-2,2',4,4',6,6’-hexanitrobiphenyl 



phosphorus oxychloride 



pyridine 



APPARATUS 



2-L Florence flask 



graduated cylinder 



thermometer 



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Megalomania's Method of Making <i>m</i>-Picrylpicryl Chloride 



water 



ra-Picrylpicryl chloride can be prepared by refluxing 75 mL of pyridine with 0.33 mole of 3-methoxy- 
2,2',4,4',6,6’-hexanitrobiphenyl suspended in 1.2 L of benzene for 1 hour at 100 °C in a round bottomed 
2-L Florence flask . Dissolve the product of the refluxing into 400 mL of phosphorus oxychloride and 
warm for 1 hour at 100 °C. Dump the whole works into ice water to precipitate the crystals of m- 
picrylpicryl chloride, filter to collect the crystals, and wash them with water . Allow the crystals to dry, 
and purify them by recrystallizing from n-hexane . A yield of 89% is obtained. You will need a graduated 
cylinder for measuring liquids, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making the Polyester Polymer 4,4-Dinitropimelyl Chloride and 2, 2-Dinitro- 1,3-Propanediol 




The Polyester Polymer 4,4-Dinitropimelyl 



Chloride and 2,2-Dinitro-1,3-Propanediol| 




A 




melting point 
180 °C 


boiling point 

? °C 


DNPA polymer 


molecular mass 
(380.32) n 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
( C 10 H 12 N 4°12)n 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 


/■ -- 




This explosive is the polymerization product of the explosive DNPA, the synthesis of which is 
described in its own lab. It has the appearance of a cream colored powder or an amber pellet when 
melted together. It is fairly stable, resisting heat and shock to a degree. I do not have much other data of 
use on this compound. I know the name of this one is pretty strange, there isn't even any chlorine in the 
final product. 





CHEMICALS 


APPARATUS 


4,4-dinitropimelic acid 


250-mL Erlenmever flask 


dioxane 


graduated cylinder 


nitrogen 


thermometer 



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Megalomania's Method of Making the Polyester Polymer 4,4-Dinitropimelyl Chloride and 2, 2-Dinitro-l, 3-Propanediol 



phosphorous pentoxide 



thionyl chloride 



water 



vacuum desiccator 



This preparation is a two-step process which first involves the synthesis of the chloride, and then the 
polyester. The chloride is prepared by very carefully refluxing a mixture of 33 mL of 4,4-dinitropimelic 
acid with 90 mL of thionyl chloride in a round bottomed 250-mL Erlenmeyer flask for 2 hours. Filter the 
mixture while still hot to collect the crystals then rapidly cool them to -15 °C. Recrystallization from 
thionyl chloride gives a 95% yield of the chloride. To polymerize the chloride, add it to 50 mL of 
dioxane for every 0. 1 moles (about 28 g) of the chloride, in a flask of suitable size. During mixing, the 
dioxane should be heated to 100 °C and the works should be under dry nitrogen . The polymerization 
will take about 173 hours. The polymer is washed with water , then vacuum steam distilled at 25 °C. The 
polymer can be dried over phosphorous pentoxide in a vacuum desiccator at a pressure of 2 mm of 
mercury. You will need a graduated cylinder for measuring liquids, and a thermometer to monitor the 
temperature. 




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Megalomania's Method of Making DNPA 












■■■hUihHibbi 




melting point 
137 °C 


boiling point 

? °C 


DNPA 


molecular mass 
250.23 g/mol 


density 
1.52 g/mL 




table key 


sensitivity 

low 


chemical formula 
C 7 Hi 0 N 2 O 8 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 


A 










o o 



DNPA is the acronym for 4,4-dinitropimelic acid, another name is 4,4-dinitro-l,7-heptanedioic acid. 
This explosive is fairly stable to heat and shock as well as being storable at room temperature. While it 
is an explosive itself, it is usually used to manufacture polynitroaliphatic explosives and propellents. It 
may be more useful to polymerize this compound into the polyester polymer 4,4-dinitropimelyl chloride 
and 2,2-dinitro-l,3-propanedio] . 



A 



CHEMICALS 


APPARATUS 


charcoal 


beaker 




ethyl ether 


graduated cylinder 




hydrochloric acid 


pipet/buret 


methvl alcohol 


stirrer/stirring rod 


methyl acrylate 




potassium dinitroethanol 


water 





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Megalomania's Method of Making DNPA 



Preparation is by two steps, the first forms the dimethyl ester of DNPA, and the second hydrolyzes it. 
In the first step, 1200 mL of methyl acrylate is added dropwise, with a pipet or buret , while stirring with 
a magnetic stirrer or stirring rod , to an aqueous solution of 2.5 moles of potassium dinitroethanol at 
room temperature inside a large beaker . The addition is completed in 3 hours with 8 more hours of 
stirring required to complete the reaction. After completion of the stirring , the ester that should have 
formed is extracted several times with ethyl ether , decolorized with charcoal , and the ethyl ether is 
removed under vacuum. The impure ester is then recrystallized from methyl alcoho . The second step 
hydrolyzes 39 g of the ester by refluxing it with 350 mL of 18% hydrochloric acid for several hours. 
After cooling, the 4,4-dinitropimelic acid is crystallized by adding water . The total yield based on 
potassium dinitroethanol is 55-56%. You will need a graduated cylinder for measuring liquids. 




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Megalomania's Method of Making EGDN 






melting point 
-22.8 °C 


boiling point 
explodes at 114 °C 


EGDN 


molecular mass 
152.06 g/mol 


density 
1.490 g/mL 




table key 


sensitivity 

high 


chemical formula 

o 2 noch 2 ono 2 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 


A 









0 " 

1 + 

0— N— O 

+ r~ 

"O-N-O 

O 



EGDN stands for ethylene glycol dinitrate, other names include 1,2-ethanediol dinitrate, glycol 
dinitrate, or nitroglycol. EGDN is almost exactly like nitroglycerin, from its chemical properties to its 
preparation. EGDN will cause severe headaches, as does nitroglycerin, but EGDN headaches are worse, 
it is also more poisonous, so wear appropriate safety gear. EGDN has better stability in comparison to 
nitroglycerin, it is also safer to manufacture and handle. The disadvantages of EGDN vs. nitroglycerin is 
its greater volatility and slower explosive velocity. EGDN was first used in France as a component in 
non-freezing dynamites. The critical precursor in this synthesis is ethylene glycol, which is the primary 
ingredient in automobile anti-freeze. 




CHEMICALS 


APPARATUS 


chloroform 


250-mL/1000-mL beaker 


ethylene glycol 


desiccator 


nitric acid 


graduated cylinder 




sodium carbonate 


litmus paper 




sodium chloride 


pipet/buret 



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Megalomania's Method of Making EGDN 



sulfuric acid 



separatory funnel 



water 



stirring rod 



thermometer 



Prepare a nitrating mixture by mixing 22 mL of concentrated sulfuric acid (>75%) and 15 mL of 
concentrated nitric acid (>75%) in a 250-mL beaker . Place the beaker into a salt-ice bath and cool it to 
under 20 °C. While monitoring the temperature with a thermometer , very slowly add 9 mL of ethylene 
glycol drop by drop with a pipet or buret , keep the temperature below 25 °C at all times. After the glycol 
addition is complete, allow the mixture to sit for 15 minutes. Next, pour the mixture into a 1000-niL 
beaker filled with 600 mL of water and stir for several minutes with a stirring rod . Pour the solution into 
a separatory funnel , allow the EGDN to settle out, it will form a layer on the bottom of the separatory 
funnel. Drain off the EGDN and keep the acid waste for further extraction. Place the EGDN back into a 
clean separatory funnel and add plenty of 38° C to 45° C water, mix, then separate. Wash the EGDN 
again, then wash with a warm 4% solution of sodium carbonate . Wash with warm water three more 
times. Give it a final wash of concentrated .odium chloride solution, let it sit one day before separating. 
Separate and check the EGDN for acidity with blue itmus paper . If it is still acidic, keep washing. It 
must be neutral or it will explode. Dry the neutral EGDN in a desiccator , this may take several days. 
You will need a graduated cylinder for measuring liquids. 

To extract any EGDN that may still be in the waste acid, first neutralize the acid with sodium 
carbonate solution. Next add an equal volume of chloroform to the neutral waste acid. Mix well then 
place it into the separatory funnel. Separate out the EGDN and let it stand in the open for one day so the 
chloroform may evaporate. Add the EGDN to the washing process above. 




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Megalomania's Method of Making FOX-7 






melting point 
238 °C (dec) 


boiling point 


FOX-7 


molecular mass 
148.1 g/mol 


density 
1.885 g/mF 


table key 


sensitivity 
very low 


chemical formula 
C 2 H 4 N 4 O 4 


explosive velocity 
8870 m/s 


estimated cost 
$0.50 /g 




FOX-7 is a code name for 1,1 -diamino-2, 2-dinitroethylene, also called 1,1 -diamino-2, 2- 
dinitroethene, and its acronyms can be either DADE or DADNE. FOX-7 is a recent development in the 
search for insensitive high explosive munitions and is the brainchild of the Swedish Defense Research 
Agency. While FOX-7 is not more powerful than existing explosives like HMX it is being considered as 
an effective replacement in certain applications because it is a much safer explosive being quite stable to 
shock, friction, and heat. It is also an inert chemical with demonstrated compatibility to the usual 
substances used in explosives. FOX-7 is currently being tested in plastic bonded explosive formulations 
with energetic binders, in propellant formulations for artillery, and is being considered as a replacement 
in composition B formulations. 

The molecular structure of FOX-7 is actually quite simple considering its performance capabilities. 
While the chemical precursors to synthesize it have been around for over 150 years, it was only in the 
mid 90’ s that the pieces were put together just right. The precursors required to synthesize FOX-7 are 
therefore somewhat easy to come by. Getting the two amino groups on an ethene backbone is quite 
impossible with straightforward synthetic techniques. A more complex nitrogen containing ring is first 
nitrated, and then the ring is broken forming both of the amines and the double bond of ethane. 









CHEMICAFS 


APPARATUS 1 




ammonium hydroxide 


addition funnel 1 



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Megalomania's Method of Making FOX-7 



2-methoxv-2-methvl-4,5-imidazolidinedione 


500-mL flask 




nitric acid 


graduated cylinder 


sulfuric acid 


stirring rod/stirrer 


distilled water 


thermometer 



The synthesis of FOX-7 proceeds in 2 stages. The first stage nitrates an imidazole type ring, and the 
second stage breaks the ring forming the final product, 1,1 -diamino-2, 2-dinitroethylene. 

Preparation of 2,2-dinitromethylene-4,5-imidazolidinedione. Place 198 mL of concentrated sulfuric 
acid (95% and up) in a 500-mL round bottomed flask and immerse the flask in a salt-ice bath to cool the 



acid. When the acid has cooled slowly add 35.4 g of -methoxy-2-methyl-4,5- 


imidazolidinedione, which 


should form a clear yellow solution. Set the flask up for magnetic stirring and 


attach 


an addition funnel. 



Slowly add 43 mL of 70% nitric acid to the flask over a period of 60 minutes while stirring. Keep the 
temperature of the mixture under 30 °C during the addition. After adding the acid, continue stirring for 
an additional 30 minutes without any cooling. The solution will change color from yellow, to deep red, 
and finally to a pale orange precipitate. Pour the contents of the flask over a filter to collect the 
precipitate and allow it to dry in the open air, or vacuum, at room temperature. Optionally the crystals 
can be washed with a few small portions of trifluoroacetic acid. This precipitate should be 2- 
(dinitromethylene)-4,5-imidazoledione in approximately 63% yield. 

Preparation of 1,1 -diamino-2, 2-dinitroethylene. Dissolve the above produced 2-(dinitromethylene)- 
4,5-imidazoledione in 120 mL of distilled water , with stirring, in a 500-mL flask or beaker. Place the 
flask in a cold water bath and cool it to below 30 °C. Add 30% ammonium hydroxide to the flask at such 
a rate as to keep the temperature between 20-30 °C. Add enough ammonium hydroxide to reach a pH of 
approximately 9. One could also use the weaker 3-4% ammonium hydroxide as found in the grocery 
store, but much larger quantities will be needed, so use an appropriately sized container. Stir the contents 
of the flask for 2 hours after adding all of the ammonia. Pour the material over a filter to collect the 
product. Thoroughly wash these crystals several times with water and allow them to dry under vacuum. 
What remains are bright yellow crystals of 1,1 -diamino-2, 2-dinitroethylene, aka FOX-7. Yield of the 
final product is around 54%. 

You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for 

mixing, and a thermometer to monitor the temperature. 



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Megalomania's Method of Making FOX-7 




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Megalomania's Method of Making Guanidine Carbonate 




A 




melting point 
267-270 °C 


boiling point 

? °C 


guanidine carbonate 


molecular mass 
180.170 g/mol 


density 
? g/mL 


table key 


sensitivity 
very low 


chemical formula 
[(NH 2 ) 2 C=NH] 2 H 2 C0 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 






I do not have any information on this compound other than how to synthesize it. Guanidine carbonate 
is a derivative of nitroguanidine, I suspect that it has similar properties. It can be toxic and its explosive 
properties are probably like ammonium nitrate, difficult to detonate and low powered. Other names 
include guanidinium carbonate; carbonic acid, compound with guanidine (1:2); bisguanidinium 
carbonate; and diguanidinium carbonate. 



A 



CHEMICALS 


APPARATUS 


ammonium carbonate 


evaporating dish 




ethyl alcohol 


2-L Llorence flask 


nitroguanidine 


thermometer 


water 





208 g of nitroguanidine , 300g of ammonium carbonate , and 1 L of water are heated together in a 2-L 
Florence flask in a water bath. The flask is set up for refluxing and with a thermomete dipping into the 



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Megalomania's Method of Making Guanidine Carbonate 



mixture. When the temperature reaches 65-70 °C, nitrous oxide escapes rapidly, and it is necessary to 
shake the flask occasionally to prevent the undissolved nitroguanidine from being carried up into the 
neck. Heat the flask as rapidly as may be done without the reaction becoming too violent. After all the 
material has gone into solution, the flask is removed from the water bath and the contents boiled under 
reflux for 2 hours. The liquid is then transferred to an waporating dish and evaporated to dryness on a 
steam or water bath. During this process all the remaining ammonium carbonate should be driven off. 
The residue is added to the smallest possible amount of cold water, filtered for the removal of any 
melamine that may have formed, and the filtrate is stirred up with twice its volume of 95% ethyl alcohol 
which causes the precipitation of guanidine carbonate. Traces of urea which will have formed remain in 
solution along with any ammonium carbonate which may have survived the earlier treatment. The 
guanidine carbonate is filtered off, rinsed with alcohol, and dried. The filtrate is evaporated to dryness, 
taken up in water, and precipitated with alcohol for a second crop. The yield is about 162 g or 90% of 
the theoretical yield. 




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Megalomania's Method of Making Nitroguanidine 




A 




melting point 
225-250 °C 


boiling point 
decomposes at 250 °C 


nitroguanidine 


molecular mass 
104.07 g/mol 


density 
1.5 g/mL 


table kev 


sensitivity 

low 


chemical formula 
H 2 NC(NH)NHN0 2 


explosive velocity 
7650 m/s 


estimated cost 

$?.00/g 





A 



O' NH 




Nitroguanidine, sometimes written as nitroguanadine, is a stable primary explosive compound. The 
explosive power and insensitivity of this chemical make it comparable to high explosives like TNT and 
a good choice for preparation if your safety skills are not fully established. Unfortunately, the 



preparation of guanidine nitrate, the main precursor for nitroguanidine, can be hampered as its 
precursors are difficult to obtain. This of course leads to the synthesis of nitroguanidine being hampered 
as well. With that aside, nitroguanidine is very simple to synthesize, requiring only sulfuric acid to react 
with. There are two crystalline forms of nitroguanidine, an alpha and a beta. Although there is little 
difference between the two forms, the alpha is the simpler to synthesize, the beta will quickly convert to 



the alpha anyway. 




CHEMICALS 


APPARATUS 




guanidine nitrate 


1000-mL beaker 




sulfuric acid 


graduated cylinder 


water 


stirrer/stirring rod 




thermometer 


/ 



In a 1000-niL beaker add 500 mL of 98% or greater sulfuric acid , then cool the flask in a salt-ice bath 
to 10°C or below. Slowly add 400 g of dry guanidine nitrate to the acid while stirring, keeping the 
temperature of the mixture below 10 °C. The mixture should have a milky appearance, allow it to stand 



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Megalomania's Method of Making Nitroguanidine 



at room temperature, while occasionally stirring, until it is homogeneous and free from crystals. This 
may require anywhere from 15 to 20 hours. After the wait, pour the mixture into a large beaker of ice 
and water , this will cause nitroguanidine to precipitate out of solution. After one hour of standing, with 
cooling in the salt-ice bath, all the crystals should have precipitated. Filter the mixture to collect the 
crystals, rinse them with water to remove any acid that may be behind, then dissolve them in 4 liters of 
boiling water. Allow the water to cool for 12 to 24 hours and the crystals should precipitate. Pour the 
water over a filter to collect the crystals, and then allow them to dry. The nitroguanidine formed can be 
stored safely and will not decompose. The yield is about 90%. You will need a graduated cylinder for 
measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the 
temperature. 




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Megalomania's Method of Making Guanidine Nitrate 




A 



melting point 


boiling point 


guanidine nitrate 


molecular mass 


density 


215-216 °C 


explodes at 230 °C 


122.08 g/mol 


0.75 g/mL 


table key 


sensitivity 

low 


chemical formula 

ch 6 n 4 o 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





Guanidine nitrate is both an explosive compound and a precursor to other explosives similar to this 
one. The one difficulty in making this compound is obtaining the main ingredient, dicyanodiamide. The 
preparation of dicyanodiamide is a long and involved process using cyanamide, which is made from 
potassium cyanide reacted with chlorine then the product is reacted with ammonia, the cyanamide thus 
produced is reacted with sulfuric acid or ammonium sulfide. I'm not exactly sure about the specifics as 
of yet. This process was developed at around 1920 or 1921. 1 do not have many specifics relating to 
explosive or chemical properties of this compound. Some legitimate uses of this compound include the 
manufacturing of trimethoprim, folic acid, sulpha guanidine, organic synthetics, photographic chemicals, 
and disinfectants. Other names for this explosive are guanidine mononitrate, and guanidinium nitrate. 







CHEMICALS 


APPARATUS 






ammonium nitrate 


1-L Florence flask 






dicvanodiamide 


thermometer 


water 





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Megalomania's Method of Making Guanidine Nitrate 



Place a mixture of 210 g of dicyanodiamide and 440 g of ammonium nitrate in a 1-L Florence flask, 

the flask is immersed in an oil bath for heating which has a hermometer in the oil. The oil bath should 
be preheated to 1 10-120 °C before placing the flask in, then it is warmed to 160 °C over 30 minutes, and 
held at this temp for 2 hours. At the end of that time the flask is removed and allowed to cool, and the 
contents are extracted on a steam bath by warming with successive portions of water . About 2 L of water 
will be needed, the hard cake of crystals will dissolve slowly, so sufficient time must be given for each 
portion of water to become saturated before it is decanted. The combined solution is filtered while hot 
for the removal of white insoluble material (that being ammeline and ammelide), concentrated to a 
volume of about 1 liter, and allowed to crystallize. There may be some crystals of guanidine nitrate 
mixed with the ammeline and ammelide, these can be re-dissolved in hot water and cooled to precipitate 
the ammeline and ammelide again, the guanidine nitrate will remain in solution. The mother liquors are 
concentrated to a volume of about 250 mL for a second crop, after the removal of which the residual 
liquors are discarded. The crude guanidine nitrate may be recrystallized by dissolving it in the least 
possible amount of boiling water and allowed to cool, or it may be dried thoroughly and used directly for 
the preparation of nitroguanidine. 




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Megalomania's Method of Making l-Phenyl-2-Nitro-l-Propene 




1 -Phenyl-2-Nitro-1 -Propene 






melting point 
64.5 °C 


boiling point 
139 °C 


1 -phenyl-2-nitro- 1 -propene 


molecular mass 
163.19 g/mol 


density 
1.277 g/mL 


table key 


sensitivity 

medium 


chemical formula 

c 9 h 9 no 2 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







no 2 

— ch=c-ch 3 


C®> 




- 



I do not have many specifics on this explosive such as sensitivity or detonation velocity. This 
procedure requires that the reactants be heated in a sealed tube, it is advisable to evacuate this tube of air 
as the expansion of heated air may cause it to burst. Also note that the boiling temperature of this 
compound is for a low vacuum pressure. This material will decompose at 177 °C. 



A 



CHEMICALS 


APPARATUS 


benzaldehyde 


500-mL Erlenmeyer flask 


isopropylamine 


graduated cylinder 


methyl alcohol 




nitroethane 




water 





l-phenyl-2-nitro-l -propene can be prepared by reacting 153 mL of benzaldehyde with 108 mL of 

nitroethane plus 13.6 g of isopropylamine in a sealed round bottomed 500-mL Erlenmeyer flask heated 
by submerging in a water bath for 2 hours. After heating the flask, allow it to cool to room temperature 
and shake, a yellow crystalline product should be obtained. The crystals are filtered to collect them and 



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Megalomania's Method of Making l-Phenyl-2-Nitro-l-Propene 



washed with water . They are then recrystallized from warm methyl alcohol . Yield is about 57%. You 
will need a graduated cylinder for measuring liquids. 




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2004 



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Megalomania's Method of Making PGDN 




melting point 
-20 °C 


boiling point 
decomposes at 30 °C 


PGDN 


molecular mass 
166.0 g/mol 


density 
1.368 g/mL 


table key 


sensitivity 

medium 


chemical formula 
CH 3 CH(0N0 2 )CH 2 (0N0 2 ) 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





ch 2 — ono 2 

CH — ONC'2 

ch 3 




/ 



PGDN is an acronym for propylene glycol dinitrate, other names include methylglycol dinitrate, and 
methylnitroglycol. This explosive is very similar to nitroglycerine in both its chemical, physical, and 
explosive properties, as well as its method of synthesis. Propylene glycol, a derivative of glycerol, is 
found in some anti-freezes, it is the active ingredient in certain ecological brands because it is non- 
poisonous. PGDN is actually safer to handle than nitroglycerin by a factor of ten, it sacrifices some 
explosive power, but the gain in stability more than offsets the loss of power. PGDN can be stored over 
long periods of time, unlike nitro, and it is difficult to freeze, where frozen nitro is especially dangerous. 
PGDN can even gel guncotton for use in smokeless powders, like nitro, and all this without the 
headaches too. 









CHEMICALS 


APPARATUS 




chloroform 


100-mL beaker 




nitric acid 


evaporation dish 




propylene glycol 


graduated cylinder 




sodium carbonate 


pipet/buret 




sulfuric acid 


separatory funnel 




water 


stirrer/stirring rod 



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Megalomania's Method of Making PGDN 



thermometer 



Prepare an acid mixture of 16 mL of 96% sulfuric acid and 14 mL of 90% nitric acit in a 100-mL 
beaker . Place the beaker into a salt-ice bath and cool it to 10 °C. Once cool, slowly add 9.6 mL of 
propylene glyco dropwise, with a pipet or buret , while stirring. Regulate the rate of addition to keep the 
temperature between 10-15 °C. The addition should take about 30 minutes. Do not let any liquid splash 
onto the walls of the beaker, it can oxidize and cause dangerous decomposition, if any red fumes are 
observed, dump the contents of the beaker down the drain with plenty of cold water. If at any time the 
temperature rises suddenly, or the temperature climbs over 20 °C, immediately dump the reaction. 
Having a bucket of ice water to dump the beaker into is advisable. After the addition, continue stirring 
for an additional 10 minutes, and maintain the temperature. Pour the contents of the beaker into a 
separatory funnel and allow it to stand for 15 minutes. The lower layer should be acid waste, draw it off 
and keep for further extraction. Leave the upper layer in the funnel, add an equal volume of cold water 
and gently shake for 1 minute. Allow the mixture to separate, the lower layer will be PGDN. Draw off 
the lower layer into a beaker, and pour the wash layer into a separate beaker. Add the PGDN back into 
the separatory funnel and wash twice more, add each wash layer to the beaker containing the first wash. 
Next, wash the PGDN with 5% sodium carbonate solution in the separatory funnel, add each of the 
carbonate washes to the beaker of the previous water washes. Test each of the carbonate washes for its 
pH, keep washing with carbonate solution until the wash is alkaline. Once the carbonate wash is alkaline, 
wash the PGDN with more water until the washes are neutral. The PGDN after the final wash may be 
cloudy from water still in it. Pour the PGDN onto an evaporation disl and let it set for 3-6 hours, the 
water should evaporate. 

To get more PGDN from the waste acid, add the acid to a separatory funnel and extract with several 
portions of chloroform . Combine all of the chloroform extractions and use it to extract the PGDN from 
the water and carbonate washes. Wash the chloroform until its pH is neutral. Allow the chloroform to 
evaporate, leaving behind PGDN which can be combined with the rest. You will need a graduated 

cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to 

monitor the temperature. 




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Megalomania's Method of Making PGDN 



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Megalomania's Method of Making Petrin Acrylate 




Petrin Acrylate 




melting point 
78 °C 


boiling point 

? °C 


petrin acrylate 


molecular mass 
325 g/mol 


density 
? g/mL 


table key 


sensitivity 


chemical formula 


explosive velocity 


estimated cost 


low 


C 8 H 11 N 3 U 11 


? m/s 


$?.00/g 





Petrin acrylate is the smaller version of pentaerythritol trinitroacrylate, or trinitroxypentaerythritol 
acrylate. Another name is pentaerythritol trinitrate monoacrylate. This substance is primarily used as a 
rocket propellent, so I guess it is not really an explosive at all. This will burn very well and will probably 
explode under the proper conditions, still, it seems to me that PETRIN, the main precursor, would make 
a more valuable explosive instead of acrylating it. Of course, one may need a suitable rocket propellent. 
This substance also acts as a very effective binder, a double plus for solid rocket fuels. 





CHEMICALS 


APPARATUS 


acrylic acid 


Erlenmeyer flask 




acrylyl chloride 


graduated cylinder 


A./V-dimethylaniline 


pipet/buret 


methyl alcohol 


thermometer 





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Megalomania's Method of Making Petrin Acrylate 



pentaerythritol trinitrate 
trifluoroacetic anhydride 
water 



Prepare a mixture of a small quantity of trifluoroacetic anhydride and glacial acrylic acid into an 
Erlenmeyer flask of suitable volume. Cool the mixture to 10-15 °C, then slowly add a small amount of 
pentaerythritol trinitrate (Petrin), with a pipe) or buret , while maintaining the temperature. Although I 
have no data for exact volumes, I suggest using equal volumes of all chemicals. After 1 hour, drown the 
mixture with water to precipitate the product. Filter the product to collect the crystals of petrin acrylate. 
Dissolve the crystals in methyl alcoho , the product is then allowed to crystallized over a period of 16 
hours at 0 °C, then washed with water to remove any trace of acidity. The final pure product is dried 
under vacuum to remove traces of solvent. The yield should be about 74%, an alternative process using 
/V,/V-dimethylaniline and acrylyl chloride instead of trifluoroacetic anhydride and acrylic acid with yields 
of 46% is possible. The high cost and difficulty using trifluoroacetic anhydride justifies the lower yield. 
You will need a graduated cylinder for measuring liquids, and a thermometer to monitor the 
temperature. 

Although petrin acrylate can be used as a propellent alone, the addition of an oxidizer can make it 
more powerful. A typical propellent composition consists of: 34.3% petrin acrylate as a binder, 1 1.8% 
triethylene glycol trinitrate as a plasticizer, 2.9% glycol diacrylate as a crosslinker, 51.0% ammonium 
perchlorate as an oxidizer, and 0.014% hydroquinone as a polymerization inhibitor. This composition is 
reported to have a specific impulse of 238 lb-sec/lb at a density of 1.3 g/mL. Plain petrin acrylate has a 
specific impulse of 214 lb-sec/lb and a burning rate of 0.2 inch/sec. 




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Megalomania's Method of Making Petrin 






melting point 
26-28 °C 


boiling point 
decomposes at 130 °C 


Petrin 


molecular mass 
271.1 g/mol 


density 
1.54 g/mL 


table key 


sensitivity 

low 


chemical formula 
H0CH 2 C(CH 2 0N0 2 ) 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







Petrin is an acronym for pentaerythritol trinitrate. One of the biggest uses for Petrin is to make petrin 
acrylate, a good propellant and binder in one, out of it. Petrin is also used as an intermediate in a number 
of other explosive nitrate esters. It has been used as a component of propellent binders, a plasticizer for 
slow burning propellents, a binder for cloud-seeding pyrotechnics, a gelling agent for nitrocellulose, and 
even in medicine as a vasodilator. There is not a lot of explosive data on Petrin because most scientists 
seem more concerned with what they can make from it instead of using it as is. What data there is comes 
from the original German patent for its synthesis back in 1937, back when the Germans were happy, 
simple country folk with religious issues and a Christian superiority complex. 



CHEMICALS 



APPARATUS 



ammonium carbonate 



beaker 



methylene chloride 



crystallization dish 



nitric acid 



graduated cylinder 



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Megalomania's Method of Making Petrin 



pentaerythritol 


pipet 




sulfuric acid 


stirrer/stirring rod 




water 


thermometer 





There are many different methods concerning the synthesis of Petrin, but perhaps the best is an 
anonymous publication from 1971. This reaction creates both Petrin and PETN. Prepare a mixture of 
pentaerythritol and 100% nitric acid in a weaker chilled to 0 °C in a salt-ice bath. Add to this mixture 
some methylene chloride solvent and mix well. Now add 2 mL of 100% sulfuric acic for every 8 mL of 
nitric acid added. The temperature must stay at 0 °C throughout the reaction. I do not have data 
concerning exact volumes, I suggest using several times the volume of mixed acid to the volume of 
pentaerythritol. After the sulfuric acid has been added, remove the methylene chloride by decanting it 
off the top with a pipet . Add more fresh methylene chloride and remove it after a few minutes of mixing. 
Continue the solvent addition and removal several times during the reaction. Combine all of the solvent 
extracts and neutralize them with ammonium carbonate until neutral to litmus paper. The neutralized 
methylene chloride can be distilled to concentrate the volume of Petrin solution while recollecting the 
methylene chloride. The remaining Petrin residue can then placed in a crystallization dish to evaporate 
the rest of the way. You could also use vacuum drying to speed the process along. Adding water to the 
remaining acid mix should precipitate the that formed, further purification instructions can be 

found on that page. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic 
stirrer for mixing, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making PETN 




PETN 




melting point 
141 °C 


boiling point 
ignites at 210 °C 


PETN 


molecular mass 
316.14 g/mol 


density 
1.773 g/mL 


table key 


sensitivity 

medium 


chemical formula 
C 5 H 8 N 4°12 


explosive velocity 
8300 m/s 


estimated cost 

$?.00/g 



ono 2 ono 2 



o 2 no 




ono 2 




PETN is an acronym for pentaerythritol tetranitrate, other names include 1,3-propanediol; 2,2-[bis- 
(nitroxy)methyl] -dinitrate; 2, 2-bis[(nitrooxy)methyl]-l, 3-propanediol (ester); 2, 2-bishydroxymethyl- 1,3- 
propanediol tetranitrate; nitropentaerythritol; niperyt; Lentrat; Hasethrol; Peritrate; Mycardol; 
Nitropenton; Pentral 80; Dilcoran-80; Terpate; Perityl; Pentritol; Pentanitrine; Prevangor; Subicard; 
Pentryate; Vasodiatol; Neo-Corovas; Pentafin; Quintrate; Pergitral; Metranil; Cardiacap; Angitet; 
dinitrate penta; niperyth; penthrit; penthrite; pentrit; nitropenta; NP; and TEN. While PETN can not be 
detonated by flame or fuse, it only burns in the open air, it is very easily detonated by shock. A blow 
from a hammer, dropping it on the floor, and using even a weak detonator will cause detonation. PETN 
was first prepared in 1894 by the German company Rneinisch Westfalalische Sprengstoff AG. PETN is 
used as the active ingredient in detonating cord, detonating cord is like a fuse that burns as fast as 
electricity flows (as fast as sound anyway, but that is only an analogy). The cord can slice a small tree in 
half from the heat, it was wrapped around prisoners of war when no shackles were handy. Anybody gets 
out of line... Ouch. PETN has also found uses in blasting caps, grenade filler, as a sometime replacement 
for RDX, mixed with plastics as a booster charge for insensitive explosives, and in medicine as a 
vasodilator. Another nifty use for it is in sheet explosive, like bed sheets, it can be used to harden and 
shape metals, wrap around objects and all sorts of wonderful things. PETN is a rather common and 
stable high explosive that is not very difficult to prepare. This lab will require white nitric acid which 
you can make and pentaerythritol, also called tetramethylol methane and 2, 2-bis(hydroxymethyl)- 1,3- 
propanediol. Pentaerythritol may have its uses in the paint industry but no use in the hands of the public. 
I have a method of synthesizing it, but it is vague. I will look for a better procedure. 







CHEMICALS 


APPARATUS | 



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Megalomania's Method of Making PETN 



acetone 


600-mL beaker 




nitric acid 


graduated cylinder 


pentaerythritol 


stirrer/stirring rod 


sodium carbonate 


thermometer 


water 





In a 600-mL beaker , add 400 mL of white nitric acid and cool to below 5°C in a salt-ice bath. White 
nitric acid is made by adding a small amount of urea to fuming nitric acid then blowing dry air into the 
acid until it is colorless. 100 g of finely ground pentaerythritol is slowly added to the acid while stirring, 
keeping the temperature below 5°C. After all of the pentaerythritol has been added, the stirring and 
cooling are continued for 15 minutes. The mixture is then dumped in about 3 L of ice water . The crude 
product that should have formed is filtered to collect it, washed with water, and submerged in 1 L of hot 
0.5% sodium carbonate solution for 1 hour. The crystals are again collected on a filter, washed with 
water, and allowed to dry. These washings are important to remove all traces of acid. To obtain a pure 
product, dissolve the crystals in hot acetone , allow to cool, then add an equal volume of water as you 
have of acetone. Filter to collect the crystals, wash with water, and allow 24 hours to dry. You will need 
a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a 
thermometer to monitor the temperature. 




Lab 


Homel Explosivesl Chemica 


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imer 


Skillsl Lab Equi 


pmentlSafetvl 


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Megalomania's Method of Making N-Perchlorylpiperidine 




N-Perchlorylpiperidine 




A 




melting point 
explodes 


boiling point 


N-perchlory lpiperidine 


molecular mass 
167.6 g/mol 


density 
? g/mL 


table key 


sensitivity 
very high 


chemical formula 

c 5 h 10 ncio 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







/ \ 

NC1G 3 









This is an extremely dangerous compound, it is very sensitive to heat, sunlight, you name it. It can be 
desensitized by adsorption on powdered alumina and it can be stored indefinitely at a balmy -80 °C. If 
your going to make this one get your super freezer ready with liquid nitrogen, otherwise be very careful. 
You do have an industrial super freezer don't ya? Umm hmm, me too. 





CHEMICALS 


APPARATUS 


ethyl ether 


bubbler 




hydrochloric acid 


400-mL Erlenmeyer flask 




perchloryl fluoride 


graduated cylinder 






piperidine 



Preparation is by reacting an aqueous solution consisting of 8.0 g of liperidine and 250 mL of water 
with perchloryl fluoride gas at room temperature in a 400-mL Erlenmeyer flask . The gas is bubbled 
through the solution for 20 minutes at a rate of 170 mL/minute, a bubblei would help increase the 
efficiency. The solution is then nitrogen purged for 10 minutes, extracted with ethyl ether , washed with a 
dilute solution of hydrochloric acid , and dried at room temperature under vacuum. Yield is about 66%. 
You will need a graduated cylinder for measuring liquids. 



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Megalomania's Method of Making N-Perchlorylpiperidine 




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Megalomania's Method of Making Perchlorates 




melting point 


boiling point 


perchlorates 


molecular mass 


density 


varies 


explodes 


varies 


varies 


table key 


sensitivity 

high 


chemical formula 
XC10 4 


explosive velocity 
varies 


estimated cost 
varies 







0 X 

1 

o=ci=o 

0 





A perchlorate is a chemical functional group, explosive more often then not, with the formula -C10 4 . 
Since so many pyrotechnic compounds seem to use a perchlorate somewhere in the mix, it seemed 
logical to have them here. Since there are so many I decided to have one page for all of them. It is easy 
to confuse perchlorates with chlorates, chlorites, and hypochlorites, their formulas are C10 4 , CIO 3 , 
C10 2 , and CIO respectively. Perchlorate salts are simply the product of a base with perchloric acid, 
although organic perchlorates exist as well. One thing perchlorates share in common is that they are 
strong oxidizers, they should be kept away from any reducible materials and excessive heat. Metal 
perchlorates tend to be more stable than organic perchlorates. One of the first perchlorate salts to be 
identified was potassium perchlorate, other salts of interest include aluminum perchlorate, ammonium 
perchlorate, barium perchlorate, cadmium perchlorate, calcium perchlorate, cobalt perchlorate, copper 
perchlorate, hydrazine diperchlorate, iron perchlorate, lead perchlorate, lithium perchlorate, magnesium 
perchlorate, manganese perchlorate, mercury perchlorate, nickel perchlorate, nitrosyl perchlorate, nitryl 
perchlorate, silver perchlorate, sodium perchlorate, strontium perchlorate, titanium tetraperchlorate, 
uranyl perchlorate, and zinc perchlorate. Some of these are mere curiosities, their chemical precursors 
will not be in the synthesis section. The usual data on safety and use of these compounds has been 
omitted as well in the interest of keeping this lab brief. 



A 



A 



aluminum perchlorate 


chemical formula 
A1(C10 4 ) 3 


melting point 
decomposes at 300 °C 


molecular mass 
325.37 g/mol 


density 
2.209 g/mL 



Set up a round-bottomed 500-mL Florence flask for refluxing and liquid addition. The top of the 



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Megalomania's Method of Making Perchlorates 



reflux condenser needs to be capped with a drying tube to protect the reaction from moisture. Heat to 
reflux some silver perchlorate in anhydrous methyl alcohol, then slowly add a solution of aluminum 
chloride in methyl alcohol drop by drop from the addition funnel. A precipitate of silver chloride will 
appear, filter the product to remove the silver chloride and heat the remaining solution at 150 °C to 
remove the methyl alcohol and crystallize the aluminum perchlorate. 





ammonium perchlorate 


chemical formula 
NH3CIO4 


melting point 
decomposes at 269 °C 


molecular mass 
117.49 g/mol 


density 
1.9518 g/mL 



Ammonium perchlorate can be prepared in the lab by carefully neutralizing perchloric acid with 
either gaseous ammonia or aqueous ammonium hydroxide. Filter the solution to collect the crystals of 
ammonium perchlorate, recrystallize them from water, and dry at 1 10 °C until a constant weight is 
obtained. 



barium perchlorate 


chemical formula 
Ba(C10 4 ) 2 


melting point 
505 °C 


molecular mass 
336.27 g/mol 


density 
3.681 g/mL 





Anhydrous barium perchlorate is prepared by heating a mixture of solid barium chloride and nitrosyl 
perchlorate, or by heating a mixture of barium carbonate and ammonium perchlorate. 





cadmium perchlorate 


chemical formula 
Cd(C10 4 ) 2 


melting point 
290 °C 


molecular mass 
311.30 g/mol 



Anhydrous cadmium perchlorate can be prepared by mixing together cadmium nitrate with 
anhydrous perchloric acid and 100% nitric acid. 





calcium perchlorate 


chemical formula 
Ca(C10 4 ) 2 


melting point 
220 °C 


molecular mass 
238.98 g/mol 



Anhydrous calcium perchlorate can be prepared by heating a mixture of 100 g of calcium carbonate 
with 235 g of ammonium perchlorate. Ammonium carbonate will be evolved as a gas, leaving behind 
pure calcium perchlorate. 





cobalt perchlorate 


chemical formula 
Co(C10 4 ) 2 


molecular mass 
257.83 g/mol 


density 
3.327 g/mL 



The hexahydrate of cobalt perchlorate can be prepared by dissolving calcium carbonate, or calcium 
oxide, in aqueous perchloric acid. Evaporation of the solution yields crystals of cobalt perchlorate. 



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Megalomania's Method of Making Perchlorates 





copper perchlorate 


chemical formula 
Cu(C10 4 ) 2 


melting point 
82.3 °C 


molecular mass 
262.43 g/mol 


density 
2.225 g/mL 



Anhydrous copper perchlorate is prepared by heating in vacuum at 200 °C a mixture of nitrosyl 
perchlorate and your choice of either copper monoxide, copper dichloride, or copper nitrate. It can also 
be prepared by reacting copper powder with nitrosyl perchlorate in an organic solvent. 





hydrazine diperchlorate 


chemical formula 
N 2 H 4 .2HC10 4 


melting point 
191 °C 


molecular mass 
232.97 g/mol 


density 
2.21 g/mL 



Hydrazine diperchlorate, or HDP, can be prepared by reacting equimolar amounts of aqueous barium 
perchlorate with hydrazine sulfate. Filter to remove the precipitate of barium sulfate, and evaporate the 
filtrate on a water bath to yield crystals of HDP. 





iron perchlorate 


chemical formula 
Fe(C10 4 ) 2 


melting point 
explodes 


molecular mass 
254.75 g/mol 



Iron perchlorate is prepared by reacting 70% perchloric acid with iron sulfide, or iron sulfate, 
followed by evaporation of the solution. Heat the solution very gently to evaporate, strong heating can 
cause an explosion. 





lead perchlorate 


chemical formula 
Pb(C10 4 ) 2 


melting point 
83 °C 


molecular mass 
406.09 g/mol 


density 
2.6 g/mL 



The trihydrate of lead perchlorate can be prepared by dissolving lead carbonate in aqueous perchloric 
acid and evaporation the solution until crystals appear. 





lithium perchlorate 


chemical formula 
Li(C10 4 ) 2 


molecular mass 
205.84 g/mol 



The trihydrate of lithium perchlorate can be prepared by reacting lithium sulfate with barium 
perchlorate in solution, then evaporating the solution to yield the crystals. It can also be prepared by 
reacting lithium carbonate with aqueous perchloric acid. 





magnesium perchlorate 


chemical formula 
Mg(C10 4 ) 2 


melting point 
224-520 °C 


molecular mass 
223.21 g/mol 


density 
2.21 g/mL 



The hexahydrate of magnesium perchlorate can be prepared by dissolving pure magnesium oxide in 
dilute perchloric acid. Evaporate the solution until fumes appear, then cool. Filter to collect the crystals 



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Megalomania's Method of Making Perchlorates 



of magnesium perchlorate that should have formed, and recrystallize them from water. 





manganese perchlorate 


chemical formula 
Mn(C10 4 ) 2 


melting point 
explodes 


molecular mass 
253.84 g/mol 



The hexahydrate of manganese perchlorate can be prepared by dissolving manganese hydroxide, or 
manganese carbonate, in dilute perchloric acid. Evaporate the solution until crystals appear. 



mercury perchlorate 


chemical formula 
Hg(C10 4 ) 2 


molecular mass 
399.49 g/mol 





Anhydrous mercury perchlorate can be prepared by adding a solution of perchloric acid in 
trifluoroacetic acid to and mercury salt in trifluoroacetic acid. Carefully evaporate the solution until 
crystals form. 





nickel perchlorate 


chemical formula 
Ni(C10 4 ) 2 


melting point 
explodes 


molecular mass 
257.61 g/mol 


density 
3.4 g/mL 



The hexaammoniate of nickel perchlorate can be prepared by adding a solution of 14 g of sodium 
perchlorate in 50 mL of water to a solution of 23.8 g of nickel dichloride and 5.4 g of ammonium 



chloride in 120 mL of water. Slowly add with stirring 60 mL of concentrated ammonium hydroxide. 
Cool this mixture for 4 hours with a salt-ice bath, then filter to collect the crystals of the perchlorate. 




Nitryl perchlorate can be prepared by distilling anhydrous perchloric acid, allowing the distillate to 
drip onto a large excess of dry dinitrogen pentoxide chilled to -80 °C (yes that's negative) and some 
nitromethane. The mixture is allowed to warm to room temperature, then kept under vacuum for 48 
hours to remove any volatile contaminants. 





potassium perchlorate 


chemical formula 
KC10 4 


melting point 
588 °C 


molecular mass 
138.55 g/mol 


density 
2.53574 g/mL 



Potassium perchlorate is prepared by slowly adding 50 mL of concentrated sulfuric acid to 2-5 g of 
potassium chlorate. The addition is slow to avoid explosion. Alternately, nitric acid, phosphoric acid, or 



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Megalomania's Method of Making Perchlorates 



chromium trioxide can be used instead of sulfuric acid. It can also be prepared by mixing potassium 
chloride and nitrosyl perchlorate in solid form and heating. A residue of potassium perchlorate will be 
left behind. 





silver perchlorate 


chemical formula 
AgC10 4 


melting point 
486 °C 


molecular mass 
207.32 g/mol 


density 
2.806 g/mL 1 



Anhydrous silver perchlorate can be prepared by adding anhydrous perchloric acid to a solution of a 
silver salt dissolved in trifluoroacetic acid. It can also be prepared by dissolving silver oxide in aqueous 
perchloric acid and evaporating the solution until crystals appear. 





sodium perchlorate 


chemical formula 
NaC10 4 


melting point 
473 °C 


molecular mass 
122.44 g/mol 


density 
2.5298 g/mL 



The monohydrate of sodium perchlorate can be prepared by dissolving sodium carbonate in a slight 
excess of dilute perchloric acid. Evaporate some of the solution, then cool to 50 °C. The solid can be 
centrifuged, collected, and dried at 250 °C. The anhydrous can be obtained by recrystallizing from water 



above 53 °C. 





strontium perchlorate 


chemical formula 
Sr(C10 4 ) 2 


melting point 
decomposes 


molecular mass 
286.52 g/mol 


density 
2.973 g/mL 



The monohydrate of strontium perchlorate can be prepared by dissolving pure strontium nitrate in an 
excess of perchloric acid, and neutralizing the acid with strontium carbonate. Centrifuge to collect waste 
solids, and chill the liquid until crystals of the perchlorate appear. 





titanium tetraperchlorate 


chemical formula 
Ti(C10 4 ) 4 


molecular mass 
445.70 g/mol 



Anhydrous titanium tetraperchlorate can be prepared by mixing 8 moles of anhydrous perchloric acid 
with 1 mole of titanium tetrachloride at -10 °C. 





uranyl perchlorate 


chemical formula 
U0 2 (C10 4 ) 2 


melting point 
90 °C 


molecular mass 
469.0 g/mol 



The hexahydrate of uranyl perchlorate can be prepared by dissolving ordinary hardware store brand 
uranium trioxide in 40% perchloric acid. Concentrate the solution on a water bath then chill to yield 
yellow crystals of the perchlorate. 



http://www.roguesci.org/megalomania/explo/perchlorates.html (5 of 6)12-8-2004 17:25:13 



Megalomania's Method of Making Perchlorates 





zinc perchlorate 


chemical formula 
Zn(C10 4 ) 2 


melting point 
106 °C 


molecular mass 
264.27 g/mol 


density 
2.252 g/mL 



The hexahydrate of zinc perchlorate can be prepared by mixing solutions of zinc sulfate and barium 
perchlorate, filtering off the precipitate of barium sulfate, and evaporating the solution until crystals 
appear. It can also be prepared by zinc oxide, or zinc carbonate, in aqueous perchloric acid and 
evaporating the solution until crystals appear. 




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Megalomania's Method of Making Nitrosyl Perchlorate 




| A 




melting point 
decomposes 


boiling point 




nitrosyl perchlorate 


molecular mass 
129.47 g/mol 


density 
2.169 g/mL 


table key 


sensitivity 

high 


chemical formula 
N0C10 4 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







This rather unstable compound should be kept away from moisture, heat, and other organic liquids 
with with it will ignite or decompose. This substance has the appearance of white crystals that pull 
moisture from the air. It will decompose on heating and will react with water forming harmful nitrogen 
oxide, NO x , compounds. This substance was first prepared in 1909 by the scientists K.A. Hoffman and 
A. vonZedtwitz. 





CHEMICALS 


APPARATUS 




nitric oxide 


bubbler 




nitrogen dioxide 


Erlenmever flask 


perchloric acid 


vacuum desiccator 


phosphorus pentoxide 





Nitrosyl perchlorate can be prepared by passing a mixture of nitric oxide gas and nitrogen dioxide gas 
into 72% perchloric acid in an Erlenmeyer flask . The use of a bubbler can increase the amount of gas 
that reacts with the acid. Evaporate the resulting mixture until the temperature rises to 140 °C and dense 
white fumes are evolved, then cool. Over times crystals will precipitate, filter to collect them. The 
product can be dehydrated in a vacuum desiccator over phosphorus pentoxide in the desiccator. 



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Megalomania's Method of Making Nitrosyl Perchlorate 




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Megalomania's Method of Making NONA 




melting point 


boiling point 


NONA 


molecular mass 


density 


decomposes at 440 °C 


— 


635.31 g/mol 


1.78 g/mL 


table key 


sensitivity 

high 


chemical formula 
C 18 H 5 N 9°18 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



0 



0 




N 



A ;; " 



,0 



0 




NONA is an acronym for nonanitroterphenyl. The more scientific names of 2, 2', 2", 4, 4', 4", 6, 6', 6"- 
nonanitroterphenyl and l,T:3',l"-terphenyl, 2,2',2",4,4',4",6,6',6"-nonanitro- have also been used. This 
substance has the appearance of light yellow crystals. Although its stability to shock and friction is not 
very high, it has good thermal stability and low volatility. This substance has found a use as a booster 
explosive in space applications. This information was classified, but now it is free. 





CHEMICALS 


APPARATUS 


copper 


500-mL Florence flask 


l,3-dichloro-2,4,6-trinitrobenzene 


funnel 


infusorial earth 


graduated cylinder 


nitrobenzene 


magnetic stirrer 



http://www.roguesci.org/megalomania/explo/NONA.html (1 of 2)12-8-2004 17:25:14 





Megalomania's Method of Making NONA 



picryl chloride 
silicic acid 
toluene 



Prepare a glassware setup for addition and refluxing with a round bottomed 500-mL Florence flask . 
Dissolve 30 g of thoroughly dried ticryl chloride in 50 mL of anhydrous nitrobenzene in the flask. 
Gently heat the solution to reflux. Prepare a mixture of 5.6 g of ,3-dichloro-2,4,6-trinitrobenzene and 
13 g of electrolytic coppei dust. This mixture will need to be constantly stirred to keep the copper in 
solution homogenous, add it from the addition funnel over a 15 minute period. Continue refluxing for an 
additional 10 minutes, then filter the solution while it is still hot. Wash the inorganic residue on the filter 
with several small portions of hot nitrobenzene. The filtrate and washings should then be concentrated 
on an oil bath under reduced pressure to a thick syrup. Add 350 mL of toluene and reflux the mixture for 
15 minutes. Filter the hot liquid, the dark brown residue, about 8 g, should be suspended in 350 mL of 
toluene , and the mixture refluxed again for 15 minutes, and filtered while hot. The residue on the filter 
should be a brown powdery solid weighing about 5.5 g after drying in air. The combined filtrates and 
washings are filtered through a 3 inch pad of silicic acid on a 90-mm sintered glass funnel , and the 
absorbent pad is washed with toluene until a bright yellow band has moved near the bottom of the filter. 
The filtrate is evaporated to dryness, the residue is added to 300 mL of toluene and refluxed for 15 
minutes and filtered. The product recovered on the funnel should be a tan crystalline material. This 
material is purified in two portions by chromatography on silicic acid- infusorial eartl , yielding about 2.0 
g of a light yellow crystalline solid that if there is any decency in the world will be NONA. You will 
need a graduated cylinder for measuring liquids, and a magnetic stirrer for mixing. 




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Megalomania's Method of Making NPN 




melting point 


boiling point 


NPN 


molecular mass 


density 


-100 °C 


110.5 °C 


105.09 g/mol 


1.0538 g/mL 


table key 


sensitivity 
very low 


chemical formula 

ch 3 ch 2 ch 2 ono 2 


explosive velocity 
5100 m/s 


estimated cost 

$?.00/g 











> 

O 

°=< 

o 


(§> 





NPN is an acronym for n-propyl nitrate, it also has the names propyl nitrate; monopropyl nitrate; 1- 
propyl nitrate; and propyl ester of nitric acid. This substance is a watery white liquid that is extremely 
toxic if inhaled. It is very stable, it can be knocked around for a good bit before detonating, but 
increasing the temperature will increase the sensitivity. This substance can be detonated while vaporized 
making it a good fuel-air explosive, The maximum detonation velocity that can be achieved is 1,900 m/s 
at 21% concentration in air. Anything more or less will have a lower velocity and is thus less powerful. 
NPN has found many uses in industry, the list includes: rocket propellent, jet motor starting fuel, turbine 
motor fuel, a degreasing solvent for iron and aluminum, and a diesel fuel additive just to name a few. 





CHEMICALS 


APPARATUS 




ethyl acetate 


stirrer/stirring rod 






isopropyl alcohol 


thermometer 


nitric acid 




n-propyl alcohol 


sodium carbonate 






sulfuric acid 



http://www.roguesci.org/megalomania/explo/NPN.html (1 of 2)12-8-2004 17:25:15 




Megalomania's Method of Making NPN 



NPN can be prepared by reacting n-propyl alcohol with 70% nitric acid dissolved in ethyl acetate . 
During the reaction the temperature must be kept at 20 °C, the product can then be extracted by 

distillation . 

NPN can also be prepared by reacting a continuous stream of pyl alcohol below the surface of a 
stirred mixed acid composed of 20% nitric acid, 68% sulfuric acid , and 12% by weight of water in an 
open stainless steel vessel cooled to 0-5 °C. Additional mixed acid is also simultaneously introduced at 
about a third of the depth of the liquid. An overflow pipe maintains a constant reactant level and the 
effluent product is separated, washed with aqueous 10% sodium carbonate solution, and dried by 
passage through a Filtrol packed tower with 50% isopropyl alcohol as the solvent at 0 °C. Yield is about 
66.5%. Sorry, I have no volumes to give you. You will need a stirring rod or magnetic stirrer for mixing 
and a hermometer to monitor the temperature. 




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Megalomania's Method of Making NTN 




melting point 
-58 °C 


boiling point 
100 °C 


NTN 


molecular mass 


density 
1.269 g/ml 


table kev 


sensitivity 

high 


chemical formula 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



X 

! 

W"/ ? x 



Y 



z 

unknown 




NTN is not an explosive compound but rather an explosive mixture. Although I don't particularly 
care about mixtures, this one intrigues me because it is a liquid explosive. This substance is a clear to 
light yellow homogeneous liquid that is somewhat sensitive to shock and friction but stable in the open 
air. 





A 




CHEMICALS 


APPARATUS 




nitromethane 






1 -nitropropane 






tetranitromethane 






NTN is composed of a mixture of 51.7% nitromethane, 33.2% tetranitromethane, and 15.1% 



nitropropane . Percentages are by weight. 



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Megalomania's Method of Making NTN 




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Megalomania's Method of Making Tetranitromethane 






melting point 
13.8 °C 


boiling point 
125.7 °C 


tetranitromethane 


molecular mass 
196.04 g/mol 


density 
1.62294 g/cc 




table key 


sensitivity 

low 


chemical formula 
C(N0 2 ) 4 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 


A 









no 2 

1 

ChW^NC^ 

0 2 N 




Tetranitromethane, also called TeNMe, is a colorless to pale yellow liquid that was first prepared by 
the action of nitric acid on trinitromethane back in 1861. The Germans used it back in WWII for an 
intermediate in making other explosives and as a substitute for nitric acid in the V-2 rocket. A pilot plant 
in New Jersey used to make tetranitromethane blew up in 1953. This compound is rather toxic, irritating 
the skin, mucous membranes and the respiratory tract. Prolonged exposure to vapors causes damage to 
the liver, kidneys, and other organs. A concentration of 0.1 ppm in the air is fatal. Mixtures of 
tetranitromethane with organic liquids tend to form more powerful explosives, but the sensitivity is 
worse. A list of mixtures has been provided. Tetranitromethane has been proposed as a chemical warfare 
agent. 



CHEMICALS 



acetic anhydride 



nitric acid 



sodium hydroxide 



sodium sulfate 



water 



APPARATUS 



addition funnel 



beaker 



Clasien adapter 



desiccator 



250-ml Florence flask 



graduated cylinder 



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Megalomania's Method of Making Tetranitromethane 



thermometer 



This reaction will produce toxic fumes, so take the necessary precautions. Measure out 21 mL of 
100% nitric acic into a round-bottomed 250-ml Florence flask . It is important to only use anhydrous acid 
and no more than the amount proscribed, any deviation will drastically lower the yield of this reaction. 
Place a Tlasien adapts on the flask and attach a thermometei on the straight arm, almost touching the 
bottom of the flask, and an addition funne on the side arm. In this instance do not use a thermometer 
adapter to connect the thermometer, there must be a gap to allow reaction gasses to escape. 

Cool the contents of the flask to 10 °C in an ice water bath. Slowly add 47.2 mL of acetic anhydride 
in portions of 0.5 mL at a time from the buret. Do not let the temperature of the mixture rise above 10 °C 
during the addition, failure to maintain the temp may result in a dangerous runaway reaction. After the 
first 5 mL of acid has been added the reaction should have calmed down enough where you can begin to 
add larger portions of 1 to 5 mL at a time with constant shaking. 

After all the acetic anhydride has been added, everything is removed from the flask. The neck of the 
flask is wiped clean with a towel, the flask is then covered with an inverted beaker , and it is now 
allowed to come up to room temperature in the ice bath. It is important to keep the flask in the ice bath 
because the reaction can still become dangerous if it is allowed to warm up too rapidly. The flask should 
be left alone for 1 week (yes, 7 days) at room temperature. 

After sitting for a week the contents are mixed with 300 mL of water in a 500-mL Florence flask. The 
tetranitromethane is removed by steam distillation , the tetranitromethane passes over with the first 20 
mL of the distillate. The lower layer of the distillate is separated, washed with dilute sodium hydroxide , 
and then water, and finally dried over anhydrous sodium sulfate in a desiccator . Yield is 14-16 g, or 
about 57-65%. Do not distill tetranitromethane by ordinary distillation means, it may explode. The 
residues of distillation are especially dangerous. Use only steam distillation, and even then be careful. 
You will need a graduated cylinder for measuring liquids. 



Explosive mixtures with organic compounds 

Tetranitromethane can be mixed with several compounds including benzene, ethylene glycol, gasoline, 
naphthalene, and toluene, but the resulting explosive may be rather sensitive to detonation. Here are 
some mixing ratios: 

• 87:13 mixture of benzene and T eNMe 

• 1:1 mixture of ethylene glycol and TeNMe 

• varying amounts of gasoline or diesel mixed with TeNMe are powerful but very sensitive, I 
suspect that the more TeNMe there is the more sensitive it will be 

• 1 mole naphthalene to 2 moles TeNMe 

• 4 moles of nitromethane to 1 mole TeNMe 

• mixing 10-40% paraffins and 60-90% TeNMe will make powerful explosives that are resistant to 
mechanical shock but detonate by explosive shock 

• mixing with toluene creates a very powerful explosive (>8000 m/s) that is more unstable than 



http://www.roguesci.org/megalomania/explo/tetranitromethane.html (2 of 3)12-8-2004 17:25:17 



Megalomania's Method of Making Tetranitromethane 



nitroglycerine 




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Megalomania's Method of Making Tetryl 




melting point 


boiling point 


tetryl 


molecular mass 


density 


130 °C 


explodes at 180°C 


287.15 g/mol 


1.57 g/mL 


table key 


sensitivity 

medium 


chemical formula 

c 7 h 5 n 5 o 8 


explosive velocity 
7260 m/s 


estimated cost 

$?.00/g 



>TCb 

N 

O2N 




no 2 





Tetryl has a variety of names including nitramine; N-methyl-N,2,4,6-tetranitrobenzenamine; N- 
methyl-N,2,4,6-tetranitroaniline; picrylmethylnitramine; picrylnitromethylamine; 2,4,6- 
trinitrophenylmethylnitramine; tetralite; and pyronite. Tetryl is a stable explosivecapablee of being 
handledreasonablyy safe, yet it is still sensitive enough to be used in blasting caps or booster charges. It 
was first developed in 1889 by the scientists Michler and Meyer and studied in some detail thereafter. It 
can be heated either in the open or in solvents causing mere decomposition, usually to picric acid. Tetryl 
is more powerful then even TNT, although the lesser stability compared to TNT makes it less attractive 
to the military. You must keep tetryl in the dark and away from the skin, it will stain skin and hair 
yellow as well as cause itching or worse. 





CHEMICALS 


APPARATUS 




benzene 


500-mL beaker 




/V./V-dimethylaniline 


500-mL Erlenmeyer flask 


ethyl alcohol 


graduated cylinder 



http://www.roguesci.org/megalomania/explo/tetryl.html (1 of 2)12-8-2004 17:25:18 




Megalomania's Method of Making Tetryl 



nitric acid 


magnetic stirrer 




sulfuric acid 


separatory funnel 




water 


thermometer 





Prepare a solution of 20 mL of /V,/V-dimethylaniline and 130 mL of 99-100% sulfuric acid in a 500- 
mL beaker placed in a salt-ice bath. Keep the temperature below 25 °C while mixing this solution. Pour 
the solution into a separatory funnel and slowly add it, drop by drop, to a 500-mL Erlenmeyer flask 
containing 160 mL of 80% nitric acid that has been previously heated to 55-60 °C. During the addition, 
stir continually with a magnetic stirrer , and maintain the temperature between 65-70 °C. The addition 
should require about 1 hour. After the addition, continue stirring and maintain the temperature at 65-70 ° 
C for an additional hour. Allow the mixture to cool to room temperature and the crystals of tetryl to 
precipitate. Decant as much of the acid as possible and drown the remaining crystals with water . Filter to 
collect the crystals and wash thoroughly with water to remove traces of acid. Add the washed crystals to 
a beaker of 240 mL of water and boil for 1 hour, continually add water to replace any that boils away, 
maintaining a constant volume. Again filter to collect the tetryl, add the crystals to a beaker and add 
enough water to cover the surface, grind these crystals to as fine a paste as possible. Add water equal to 
twelve times the weight of the crystals and boil for 12 hours. Repeat this with a fresh batch of water and 
boil for another 4 hours. Filter to collect the crystals and allow them to dry. After drying, add just 
enough benzene to dissolve the crystals then filter to remove any undissolved impurities. Allow the 
benzene to evaporate then recrystallize the tetryl residue from ethyl alcohol . You will need a graduated 
cylinder for measuring liquids, and a t hermometer to monitor the temperature. 




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Megalomania's Method of Making TNO 




A 



melting point 


boiling point 


TNO 


molecular mass 


density 


decomposes at 313 °C 


— 


420 g/mol 


? g/mL 


table key 


sensitivity 

low 


chemical formula 

c 14 h 8 n 6 o 10 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





0 0 
c? v b 

OiN NH NH NCb 

0 0 
/ \ 
NCy N0 2 







TNO stands for 2,4,2,4-tetranitro-oxanilide. This substance is fairly stable, being able to resist shock, 
friction, and heat. It is primarily used as a component in pyrotechnical devices or in gunpowder 
formulations. It was first prepared in 1892 when A.G. Perkins heated oxanilide powder in nitric acid. I 
believe this lab procedure hails from an anonymous work in 1971. 



A 



CHEMICALS 


APPARATUS 




acetone 


500-mL Florence flask 


ethyl alcohol 


graduated cylinder 


nitric acid 


stirrer/stirring rod 


oxanilide 


thermometer 






water 



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Megalomania's Method of Making TNO 




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Measure out 100 mL of 98% nitric acic into a round bottomed iOO-mL Florence flask . Place the flask 
into a salt-ice bath to provide cooling. While stirring rapidly, slowly add 50 g of oxanilide while the 
temperature is maintained below 40 °C. After the addition of the oxanilide is completed (addition should 
take 2.5-3 hours), the agitation is continued for 10-15 minutes. The flask is now transferred to a water 
bath where the temperature is then raised to 80 °C over a period of 1 hour and maintained at 80-85 °C 
for 3 hours. The acid slurry is then cooled to room temperature and drowned by pouring over cracked 
ice. The product is filtered on a Buchner funnel and washed with water until it is almost acid free. The 
filter cake is placed in a beaker and sufficient water added to form a slurry. Steam is run into the slurry 
under agitation for 10 minutes. The slurry is filtered and the residue washed. The latter treatment of the 
slurry is repeated until the wash water is found to be neutral to litmus paper. The TNO is washed with 
ethyl alcohol , then acetone , dried in the air, and finally dried at 100-1 10 °C. Yield is 90-97% of the 
theoretical. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer 
for mixing, and a thermometer to monitor the temperature. 



COMM 



http://www.roguesci.org/megalomania/explo/TNO.html (2 of 2)12-8-2004 17:25:19 




Megalomania's Method of Making TNPEN 




melting point 


boiling point 


TNPEN 


molecular mass 


density 


104.5 °C 


ignites over 104 °C 


318.16 g/mol 


1.25 g/mL 


table kev 


sensitivity 

medium 


chemical formula 
(0 2 N) 3 C 6 H 2 0CH 2 CH 2 (0N0 2 ) 


explosive velocity 
appx 6000 m/s 


estimated cost 

$?.00/g 





no 2 

ono 2 

o 2 n'^^'^no 2 


c®> 





TNPEN is an acronym for B-(2,4,6-trinitrophenoxy) ethanol nitrate, also called 2,4,6- 
trinitrophenoxyethyl nitrate; or glycoltrinitrophenylether nitrate. TNPEN was first prepared by H.A. Lewis 
back in 1925, others have since revised the method, with this particular preparation developed by R.C. 
Elderfield in 1943. TNPEN will ignite when heated in the open and will detonate if struck as if by a 
hammer, so its stability is not that low, compared to TNT it is as stable and has 122% the explosive power. 
There is some conflicting data that indicates the stability may be lower. The recommended uses of this 
explosive are in detonators or boosters, and as an ingredient in propellents. The detonation velocity ranges 
from 5500 m/s to 6600 m/s depending on the density which can range from 1.15 g/mL to 1.6 g/mL 





CHEMICALS 


APPARATUS 




acetone 


beaker 




B-(2,4-dinitrophenoxv) ethanol 


250-mL Florence flask 




ethvl alcohol 


graduated cvlinder 


nitric acid 


glass filter paper 


sulfuric acid 


stirrer/stirring rod 


water 


thermometer 



http://www.roguesci.org/megalomania/explo/TNPEN.html (1 of 2)12-8-2004 17:25:20 






Megalomania's Method of Making TNPEN 



Prepare a solution of 10 g of B-(2,4-dinitrophenoxy) ethanol in 55 mL of 94% sulfuric acid in a small 
beaker . Prepare a second solution of 21.5 mL of sulfuric acid, 13.2 mL of nitric acid , and 15.7 mL of 
water in a round bottomed 150-mL Florence flask , chill this solution to between 0-10 °C with a salt-ice 
bath. It does not matter what concentration of acids are mixed so long as the total water content comes out 
to 15.7 mL. While stirring, slowly add the B-(2, 4-din itrophenoxy) ethanol solution to the cold acid mix. 
When the addition is complete, the temperature is raised in 30 minute intervals to 20 °C, 30 °C, 40 °C, 60 ° 
C, and in a 15 minute interval to 70 °C. After chilling, the cream-colored crystals are filtered using glass 
filter paper , washed free of acid, and recrystallized by dissolving in acetone and adding ethyl alcohol . You 
will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a 
thermometer to monitor the temperature. 




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Megalomania's Method of Making TNPht 






melting point 
78 °C 


boiling point 

? °C 


TNPht 


molecular mass 
257.16 g/mol 


density 
1.5 g/mL 




table kev 


sensitivity 

medium 


chemical formula 
C 8 H 7 N 3°7 


explosive velocity 
6880 m/s 


estimated cost 

$?.00/g 


A 











TNPht is also known as ethyl picrate; aethyl-[2,4,6-trinitrophenyl]-ather; pikrinsaureaethylather, or 
aethylpikrat in German; keineyaku, or keyneyaku in Japanese. The proper scientific name for this 
substance is 2,4,6-trinitrophenetole. This explosive is almost as powerful as TNT but its sensitivity is not 
all that great. This explosive would be classified as a booster, it needs a detonator to set it off and then it 
would set off a high explosive. This material was tested in France during WWI in shells as a bursting 
charge. The Japanese used it during WWII as a substitute for TNT because they had a shortage of 
toluene. This lab was developed by L. Desvergnes around 1922. 





CHEMICALS 


APPARATUS 




2,4-dinitrophenetole 


500-mL beaker 




nitric acid 


graduated cylinder 




sulfuric acid 


stirrer/stirring rod 




water 


thermometer 



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Megalomania's Method of Making TNPht 



Dissolve 53 g of 2,4-dinitrophenetole in 95 mL of 95-98% sulfuric acid in a 500-mL beaker while 
stirring. Add 62% nitric acid so that the temperature rises rapidly to 30 °C. Continue the addition, while 
maintaining the temperature between 30-40 °C by cooling with a salt-ice bath, until a total of 30 mL of 
nitric acid has been added. Pour the resulting yellow slurry into about 1500 mL of cold water , filter to 
collect the crystals, wash the crystals with cold water, and dry. There should be about 61.8 g of product, 
or 96% of the theoretical yield. You will need a graduated cylinder for measuring liquids, a stirring rod 
or magnetic stirrer for mixing, and a thermomete] to monitor the temperature. 




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Megalomania's Method of Making Trinitroanisol 




Trinitroanisol 






melting point 
67 °C 


boiling point 
decomposes at 165 °C 


trinitroanisol 


molecular mass 
243.13 g/mol 


density 
1.60 g/mL 


table key 


sensitivity 

high 


chemical formula 

c 7 h 5 n 3 o 7 


explosive velocity 
7640 m/s 


estimated cost 

$?.00/g 





och 3 



o 2 n- 



■no 2 



no 2 




Trinitroanisol, also known as 2,4,6-trinitroanisol; 2,4,6-trinitrophenyl methyl ether; and methyl 
picrate, is a somewhat sensitive explosive compound similar to picric acid, with the exception that it 
does not form dangerous salts with metals. It is stable at elevated temperatures, being meltable, but it is 
detonated by shock and friction. The melting point of this compound is rather low which helps when 
filling shells and blasting caps, but I would not recommend melting explosives at all unless you know 
what you are doing. Trinitroanisol was first prepared back in 1849 by one Dr. Cahours via the direct 
nitration of anisol, the du Pont and Maxim companies were the first to suggest using it as an explosive 
around 1904. Trinitroanisol say heavy use during WWI, but due to its tenancy to change to picric acid 
acid from moisture in air, it was used only sparingly by WWII. Other methods of preparation include the 
interaction of methyl iodide and silver picrate, the nitration of anisic acid, and of course the method 
developed by Dr. Jackson in 1898 listed below. Trinitroanisol is highly toxic! Symptoms of poisoning 
include headache, weakness, loss of appetite, gastric disturbance, and irritation of the mucous membrane 
of the upper respiratory tract. Contact with skin can cause redness, peeling, and blistering. Wear 
protective clothing and respirators at all times if possible. 









CHEMICALS 


APPARATUS 




hydrochloric acid 


50-mL beaker 



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Megalomania's Method of Making Trinitroanisol 



methvl alcohol 


500-mL Florence flask 




picryl chloride 


graduated cylinder 


sodium hydroxide 


stirrer/stirring rod 


water 


thermometer 



Add 35 g of picryl chloride to 400 mL of methyl alcohol in a round-bottomed 500-mL Florence flask . 

Set this flask up for refluxing and reflux until all of the picryl chloride has dissolved, then allow the 
solution to cool to 30-35 °C. Prepare a solution of 23 g of sodium hydroxide and 35 mL of water in a 50- 
mL beaker . Slowly pour the sodium hydroxide solution into the flask through the reflux condenser, 
allow the mixture to cool if it begins to boil before adding more. Allow the flask to sit for 1-2 hours, red 
crystals should have precipitated. Filter the mixture to collect the crystals, wash them with methyl 
alcohol, and stir into a small beaker of water. Slowly add concentrated hydrochloric acid to the beaker 
until the red color disappears. A precipitate of yellow or white crystals should form. Filter these crystals 
to collect them, wash with water to remove sodium chloride, allow to dry, then recrystallize the crystals 
from methyl alcohol. You will need a graduated cylinder for measuring liquids, a stirring rod or 
magnetic stirrer for mixing, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making Trinitrobenzene 






melting point 
122.5 °C 


boiling point 


trinitrobenzene 


molecular mass 
213.11 


density 
1.76 g/cc 


table key 


sensitivity 
very low 


chemical formula 

c 6 h 3 n 3 o 6 


explosive velocity 
7000 m/s 


estimated cost 

$?.00/g 





O2N ^^.no 2 




no 2 





1,3,5-trinitrobenzene, also known as sym-trinitrobenzene; s-trinitrobenzene; trinitrobenzeen; 
trinitrobenzene; trinitrobenzol; benzite; Rcra waste number U234; or just TNB, is a stable high explosive 
compound with slightly greater explosive force than TNT. There are two other isomers of 
trinitrobenzene, namely 1,2,4- and 1,2,3- , but they are less stable and harder to form. Trinitrobenzene is 
very poisonous, causing severe skin irritation, so it is best to use every precaution when handling it. The 
good qualities of trinitrobenzene are its high stability, great explosive power, and low sensitivity to 
friction and impact. On the down side, this procedure is not exactly an economical choice since it uses 
perfectly good TNT as the main ingredient. This procedure is a variant of the original that dates back to 
1893 when the German scientists Tiemann, Claus, and Becker observed that trinitrotoluene can be 
oxidized with nitric acid to trinitrobenzoic acid, and the latter being readily decarboxylated to form sym- 
trinitrobenzene: 



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Megalomania's Method of Making Trinitrobenzene 



CH'; 



O iff 




HO V© 

■c- 



N0 2 



0 2 N ^\/N0 2 °2 n 



trinitrotoluene 



N0 2 

trinitrob enzoic acid 



N0 2 

1,3,5 -trinitrob enzene 



This lab substitutes sulfuric acid and a chromium compound for nitric acid, the reaction is the same 
either way. There are other methods of forming TNB but this procedure is the easiest and has the highest 
yield. 



CHEMICALS 



APPARATUS 



sodium dichromate 



500-mL beaker 



sulfuric acid 



small beaker 



trinitrotoluene 



graduated cylinder 



water 



stirrer/stirring rod 



thermometer 



Prepare a mixture of 30 g of purified trinitrotoluene and 300 mL of 95-100% »uli ric acid in a tall 
500-mL beaker . Slowly add, with stirring, powdered sodium dichromate in small portions, do not allow 
any lumps to form or powder to rise to the surface. When the temperature of the mixture reaches 40 °C, 
place the baker into a cold water bath. Continue adding dichromate, while stirring, until a total of 45 g 
has been added, maintain the temperature between 40-50 °C at all times. After the addition, continue 
stirring and maintaining the temperature between 40-50 °C for 2 hours. After this time, allow the 
mixture to cool undisturbed to room temperature over a 12 hour period. Crystals of trinitrobenzoic acid 
should have formed. Decant off as much of the acidic liquid as possible, then drown the crystals in 
water . Lilter the crystals to collect them, wash with cold water, then transfer them to a miall beaker . Add 
just enough 50 °C water to dissolve the crystals. Lilter this solution hot to remove any undissolved 
impurities, then boil it until no more crystals precipitate. Allow the solution to cool, filter to collect the 
crystals, then wash them with water. These should be colorless to greenish yellow crystals of 
trinitrobenzene. Y ou will need a graduated cylinder for measuring liquids, a stirring rod or magnetic 
stirrer for mixing, and a thermometer to monitor the temperature. 



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Megalomania's Method of Making Trinitrobenzene 




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Megalomania's Method of Making Trinitrotoluene 




A 





melting point 
80.1 °C 


boiling point 
ignites at 295 °C 


trinitrotoluene 


molecular mass 
227.13 g/mol 


density 
1.654 g/mL 




table kev 


sensitivity 
very low 


chemical formula 

c 7 h 5 n 3 o 6 


explosive velocity 
7028 m/s 


estimated cost 

$?.00/g 


A 










A 



2,4,6-trinitrotoluene, or just TNT, is the oft used military and industrial explosive that may be the 
among the best recognized explosive around. Other names for TNT include: trinitrotoluol; sym- 
trinitrotoluene; a-trinitrotoluol; 2-methyl- 1,3, 5 -trinitrobenzene; entsufon; 1 -methyl-2, 4,6- 
trinitrobenzene; methyltrinitrobenzene; tolite; trilit; s-trinitrotoluene; s-trinitrotoluol; trotyl; sym- 
trinitrotoluol; alpha-trinitrotoluol; tolite; triton; tritol; trilite; tri; tutol; trinol; fiillpulver 1902; Fp02; 
tritolo; trillit; tolita; tol; and trotil. TNT was first synthesized in 1863 by a scientist named Wilbrand who 
treated toluene with sulfuric and nitric acid at near boiling temperatures. Although there are several 
isomers of trinitrotoluene, only the 2,4,6- isomer is of importance. Pure TNT is in the form of small 
columns or needles and is insoluble in water. It is quite stable, being meltable ,or able to act like a plastic 
at around 50 °C. TNT can even be boiled although the experiments did this under reduced pressure 
(50mm Hg) to lower the boiling point to around 245 °C. The normal detonation temperature is 333 °C, 
the calculated boiling point at normal atmospheric pressure is 345 °C, so don't do it. Some experiments 
have determined that the presence of foreign material like 1.9% of Fe 2 03 will lower the amount of time 
it takes for TNT to explode once it reaches its critical temperature, or 295 °C, the temperature at which 
decomposition begins. Also, mixing pure sulfur with TNT will lower the initiation temperature and 
increase the explosive power. For example, pure TNT explodes at 333 °C, 5% sulfur explodes at 304 °C, 
10% sulfur at 294 °C, 20% sulfur at 284 °C, and 30% sulfur at 275 °C. The increase in explosive power 
is gained through the addition of 5-10% sulfur. Because the stability of TNT is so great, it is harder to 



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Megalomania's Method of Making Trinitrotoluene 



detonate it, the sensitivity increases somewhat above 80° C, but is still rather low even when molten. A 
powerful blasting cap, or booster charge, will be needed to detonate TNT. This lab is carried out in three 
separate operations, forming mononitrotoluene, then dinitrotoluene, and finally trinitrotoluene. 





CHEMICALS 


APPARATUS 




ethyl alcohol 


100/500/600-mL beaker 




nitric acid 


Buchner funnel 




sodium bisulfite 


graduated cylinder 




sulfuric acid 


pipet/buret 


toluene 


separatory funnel 


water 


stirrer/stirring rod 








thermometer 



Prepare a nitrating solution of 160 mL of 95% sulfuric acid and 105 mL of 75% nitric acid in a >00- 
mL beaker set in a salt-ice bath. Mix the acids very slowly to avoid the generation of too much heat. 
Allow the mixture to cool to room temperature. The acid mixture is slowly added dropwise, with a )ipet 
or buret , to 1 15 mL of toluene in a 600-mL beaker while stirring rapidly. Maintain the temperature of 
the beaker during the addition at 30-40 °C by using either a cold water or salt-ice bath. The addition 
should require 60-90 minutes. After the addition, continue stirring for 30 minutes without any cooling, 
then let the mixture stand for 8-12 hours in a separatory funnel . The lower layer will be spent acid and 
the upper layer should be mononitrotoluene, drain the lower layer and keep the upper layer. 

Dissolve one-half of the previously prepared mononitrotoluene and 60 mL of 95% sulfuric acid in a 
500-mL beaker set in a cold water bath. Prepare a nitrating solution of 30 mL of 95% sulfuric acid and 
36.5 mL of 95% nitric acid in a 100-mL beaker. Preheat the beaker of mononitrotoluene to 50 &Deg;C. 
Very slowly add the nitrating acid to the beaker of mononitrotoluene, with a pipet or buret, drop by drop 
while stirring rapidly. Regulate the rate of addition to keep the temperature of the reaction between 90- 
100 °C. The addition will require about 1 hour. After the addition, continue stirring and maintaining the 
temperature at 90-100 °C for 2 hours. If the beaker is allowed to stand, a layer of dinitrotoluene will 
separate, it is not necessary to separate the dinitrotoluene from the acid in this step. 

While stirring the beaker of dinitrotoluene, heated to 90 °C, slowly add 80 mL of 100% fuming 
sulfuric acid, containing about 15% S0 3 , by pouring from a beaker. Prepare a nitrating solution of 40 

mL of 100% sulfuric acid, with 15% S0 3 , and 50 mL of 99% nitric acid. Very slowly add the nitrating 
acid to the beaker of dinitrotoluene, with a pipet or buret, drop by drop while stirring rapidly. Regulate 
the rate of addition to keep the temperature of the reaction between 100-115 °C. It may become 



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Megalomania's Method of Making Trinitrotoluene 



necessary to heat the beaker after three-quarters of the acid has been added in order to sustain the 100- 
115 °C temperature. The addition will require about 90-120 minutes. Maintain the stirring and 
temperature at 100-115 °C for 2 hours after the addition is complete. Allow the beaker to sit undisturbed 
for 8-12 hours, it should form a solid mass of trinitrotoluene crystals. Pour the contents of the beaker 
over a kic liner funne without any filter paper to collect the bulk of the crystals, save the acidic filtrate 
as well. Break up the collected crystals and wash them with water to remove any excess acid. Add the 
collected acid and wash filtrates to a large volume of water, this will cause any remaining trinitrotoluene 
to precipitate. Decant off as much of the water as possible and combine these crystals with the previous 
ones on the funnel. Drown the crystals in a large volume of water, filter to collect them, and wash 
several times with water. Wash the crystals by adding them to a beaker of water, heat the water enough 
to melt the crystals while stirring rapidly. Repeat the melting and stirring with a fresh batch of water 
three or four times to wash thoroughly. After the last washing, the trinitrotoluene is granulated by 
allowing it to cool slowly under hot water while the stirring is continued. Filter to collect the crystals and 
allow to dry. The TNT can be further purified by recrystallizing from ethyl alcohol , dissolve the crystals 
in 60 °C and allow the solution to cool slowly. A second method of purification is to digest the TNT in 5 
times its weight of 5% sodium bisulfite solution heated to 90 °C while stirring rapidly for 30 minutes. 
Wash the crystals with hot water until the washings are colorless, then allow the crystals to granulate as 
before. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for 
mixing, and a hermometer to monitor the temperature. 




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Megalomania's Method of Making Tris[l,2-Bis (Difluoramino)-Ethyl] Isocyanurate 




ris[1,2-Bis (Difluoramino)-Ethyl] Isocyanurate 




melting point 
48 °C 


boiling point 
? °C 


tris[ 1 , 2 -bis (difluoramino)-ethyl] isocyanurate 


molecular mass 
519.261 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
C 9 H 9 N 9 O 3 F 12 


explosive velocity 
? m/s 


estimated cost 

$?. 00 /g 





This explosive seems somewhat complected to synthesize because of the necessity for a pressurized reaction 
vessel, it can be done however. This material is insensitive to friction and heat as well as being rather hard to 
detonate from shock. This substance has found uses as both an explosive and as a rocket propellent. One of the 
nifty things about this material when it is being used as a propellent is the ability for the motor to be stopped and 
restarted when needed, this is usually the domain of liquid propellents. 





CHEMICALS 


APPARATUS 


chloroform 


graduated cylinder 


tetrafluorohvdrazine 


thermometer 


trivinyl isocyanurate 





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Megalomania's Method of Making Tris[l,2-Bis (Difluoramino)-Ethyl] Isocyanurate 



Preparation is by reacting all uorohydrazim under an initial pressure of 13.6 atm with 3 g of trivinyl 
isocyanurate in 75 mL of chloroform . The mixture is then heated to 125 °C and the reaction is continued at this 
temp for 32 minutes at a pressure of 20.75 atm. At the end of the 32 minutes the reaction vessel is cooled, vented, 
and the chloroform is distilled off. You will need a graduated cylinder for measuring liquids, a thermometer to 
monitor the temperature, and a steel reaction vessle capable of holding well over 21 atm of pressure. This is not 
your standard lab item. 




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January 31, 2004 



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Megalomania's Method of Making Trinitrostilbene 




Trinitrostilbene v 






melting point 
158 °C 


boiling point 


trinitrostilbene 


molecular mass 
159 g/mol 


density 
? g/mL 


table key 


sensitivity 

unknown 


chemical formula 

c 14 h 9 n 3 o 6 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







no 2 

OjN — ^ ^ CH — CH ^ ^ 

no 2 


<■‘1 





I do not have much information about this explosive other than how it can be prepared. This has been 
include as an informational curiosity only. Since I do not have any safety information, assume it is very 
sensitive. I suspect it has similar properties to TNT. 





CHEMICALS 


APPARATUS 




benzaldehyde 


1 00-mL beaker 




benzene 


100-mL Florence flask 




ethyl alcohol 


graduated cylinder 


piperidine 




trinitrotoluene 



Prepare a solution of 10 g of trinitrotoluene and 25 mL of benzene in a round-bottom )-mL 
Florence flask . Add 6 mL of benzaldehyde and 0.5 mL of piperidine to this solution and reflux for 30 
minutes on a steam bath. After refluxing, pour the still hot liquid into a 00-mL beaker and allow to 



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Megalomania's Method of Making Trinitrostilbene 



cool. Crystals of trinitrostilbene should begin to precipitate, once they are done filter to collect them and 
wash with twice with ethyl alcohol . Recrystallize the trinitrostilbene from a mixture of two parts ethyl 
alcohol and one part benzene. Filter the bright yellow crystals to collect them, and allow to dry. You will 
need a graduated cylinder for measuring liquids. 




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Megalomania's Method of Making l,l,l-Trinitro-2-Propyl Acrylate 




1,1,1-Trinitro-2-Propyl Acrylate 






melting point 

? °C 


boiling point 
50-60 °C 


l,l,l-trinitro-2-propyl acrylate 


molecular mass 
249.16 g/mol 


density 
? g/mL 


table key 


sensitivity 

medium 


chemical formula 

c 6 h 7 n 3 o 8 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







(N0 2 ) 3 y 

7 0 


<S> 







I have not listed any volumes for the reactants involved in this substance because I do not have any. I 
suggest using a few milliliters or grams of each in equal proportions and an excess of water for the 
hydrolyzing step. l,l,l-trinitro-2-propyl acrylate will detonate from shock and deflagrates (explodes but 
with less power) when heated. This material has the appearance of a pale yellow liquid. Note that the 
boiling temperature is in a near vacuum, not in standard atmospheric pressure. This lab was published 
anonymously in 1952. 



A 



CHEMICALS 


APPARATUS 




acrvlvl chloride 


500-mL Erlenmeyer flask 


aluminum chloride 


graduated cylinder 


carbon tetrachloride 


separatory funnel 


paraldehyde 




sodium bicarbonate 


sodium chloride 


trinitromethane 


water 



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Megalomania's Method of Making l,l,l-Trinitro-2-Propyl Acrylate 



Preparation is by refluxing for 30 minutes a mixture of trinitromethane , paraldehyde , and acrylyl 
chloride all dissolved in 50 mL of carbon tetrachloride with a little aluminum chloride added in. The 
reacted mixture is then hydrolyzed by adding water . The mixture will separate into two layers, the top is 
water and the bottom is carbon tetrachloride. Transfer the mixture to a separatory funnel and collect the 
bottom layer in a 500-mL Erlenmeyer flas . This carbon tetrachloride layer is neutralized with sodium 
bicarbonate solution, check with litmus to be sure. The neutral solution needs to be dried by pouring it 
into a clean separatory funnel then shaking with a saturated sodium chloride solution. Collect the bottom 
layer and vacuum distil the solution, the fraction that boils over is the explosive. The yield is about 
25%. You will need a graduated cylinder for measuring liquids. 




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31,2004 



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Megalomania's Method of Making Trinitromethane 




4 



melting point 
15 °C 


boiling point 
decomposes at 25 °C 


trinitromethane 


molecular mass 
151.04 g/mol 


density 
1.469 g/mL 


table key 


sensitivity 

low 


chemical formula 
CH(N0 2 ) 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



A 



no 2 



A 



o 2 n no 2 



A 



Trinitromethane, also called nitroform or TNMe, is typically used as an intermediate in the 
manufacture of other explosive compounds. It was first prepared by the action of concentrated nitric acid 
on acetylene back in 1900 or so. The Germans experimented with this process on a large scale in WWII 
for TNMe as intermediates for other explosives. The Hercules Powder Co. has a trademark they call 
Nitroform®, it is an agricultural product designed to release nitrogen into soil, it is not trinitromethane. 
Since TNMe is very acidic, it tends to form various neutral explosive salts. Most of the salts are used as 
propellants or are too unstable to use. TNMe has 137% of power vs. TNT. Keep this compound stored in 
a sealed glass container at 0 °C. 



A 



CHEMICALS 


APPARATUS 


ethyl ether 


1000-mL Florence flask 


hydrogen chloride gas 


glass filter paper 


hydrogen peroxide 


graduated cylinder 


methyl alcohol 


stirrer/stirring rod 




potassium hydroxide 


thermometer 


tetranitromethane 





/ 





























































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Megalomania's Method of Making Trinitromethane 



Prepare a solution of 168 g of potassium hydroxide in 350 mL of water in a round-bottomed 000- 
mL Florence flask , and cool to 5 °C with a salt-ice bath. While stirring, add 108 mL of 30% hydrogen 
peroxide to the solution. Next, add 117 mL of tetranitromethane at a rate which keeps the temperature at 
20-25 °C, add while stirring. The temperature is then allowed to rise to 30 °C over 15 minutes. The 
bright yellow solid, that should have formed, is filtered to collect it using 3 ass filter paper because of its 
high acidity, washed with anhydrous methyl alcohol , then anhydrous ethyl ether , and finally air dried to 
give 100% of the potassium salt of trinitromethane. The salt is suspended in anhydrous ethyl ether and 
anhydrous ydrogen chloride gas is passed in until the yellow color disappears. The white precipitate of 
potassium chloride is filtered off and washed with anhydrous ethyl ether. The ethyl ether is evaporated 
from the filtrate and additional washings at reduced pressure give 85-90% of crude trinitromethane 
which can be purified by sublimation. You will need a graduated cylinder for measuring liquids, a 
stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making Trinitro-<i>m</i>-Cresol 




Trinitro-/r>Cresol 






melting point 
107 °C 


boiling point 
decomposes at 200 °C 


trinitro-ra-cresol 


molecular mass 
243.14 g/mol 


density 
? g/mL 




table key 


sensitivity 

medium 


chemical formula 

c 7 h 5 n 3 o 7 


explosive velocity 
6850 m/s 


estimated cost 

$?.00/g 


A 













2,4,6-trinitro-ra-cresol, or just trinitrocresol, is a rarely used explosive compound similar to picric 
acid in its chemical and physical properties. The only difference from picric acid is the addition of a 
methyl group to the benzene ring. This explosive has been developed most heavily by the French, they 
call it Cresilite. Trinitrocresol is best used as a booster explosive or a primary explosive mixed with 
other more sensitive compounds. 



CHEMICALS 



APPARATUS 



777-cresol 



100-mL Florence flask 



nitric acid 



graduated cylinder 



sulfuric acid 



thermometer 



water 



Prepare a mixture of 20 mL of in - cresol and 33 mL of 99% sulfuric acic in a round-bottomed 
Florence ask . Reflux the contents of the flask for 6 hours at 120 °C. After refluxing, slowly add 40 mL 



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Megalomania's Method of Making Trinitro-<i>m</i>-Cresol 



of 52% nitric acid . During the addition, and for 3 hours afterward, keep the temperature at 100 °C by 
cooling and heating as necessary. After the 3 hours, cool the flask to 90 °C over a period of 20 minutes, 
then cool it to 70 °C over a period of 1 hour. Use either compressed air blowing into the liquid, or a salt- 
ice bath to regulate the temperature. Next, allow the flask to sit undisturbed for 12-15 hours where it can 
assume room temperature and begin to crystallize the trinitrocresol. After sitting, decant of as much of 
the acid as possible and drown the remaining crystals with water . Quickly filter to collect the crystals, 
wash them with a small amount of cold water. You should have yellow-brown crystals of trinitro-m- 
cresol. You will need a graduated cylinder for measuring liquids, and a thermometer to monitor the 
temperature. 




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Megalomania's Method of Making 2,4,6-Trinitro-<i>m</i>-Phenylenediamine 




2,4,6-Trinitro-m-Phenylenediamine 




melting point 
280 °C 


boiling point 
decomposes at 301 °C 


2,4,6-trinitro-m-phenylenediamine 


molecular mass 
243.14 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
C 6 H(N0 2 ) 3 (NH 2 ) 2 


explosive velocity 
? m/s 


estimated cost 
$?.00/g 





2,4,6-Trinitro-m-Phenylenediamine is very similar to TNT in both its explosive properties and chemical 
structure. This substance has gone by the name of 2,4,6-trinitro-l,3-diaminobenzene; 2,4,6- 
trinitrophenylenediamin-(l,3) in German; and 2,4,6-trinitrometaphenylenediamin in French. It was first 
prepared in 1884 by E. Nolting and A. Collin from esters of styphnic acid and ammonia. Many other procedures 
were tried over the years with different starting compounds until C.F. van Duin and B.C.R. van Lennep 
compiled all the others data around 1920 and developed the lab that I have reproduced here. 



CHEMICALS 


APPARATUS 


ammonium hydroxide 


200-mL beaker 


ethyl alcohol 


graduated cylinder 


trinitro-m-anisidine 


stirrer/stirring rod 


trinitro-m-phenetidine 




water 





Mix 10 g of finely pulverized trinitro-m-anisidine (or trinitro-m-phenetidine) with 80 mL of 24% ammonium 

hydroxide in a 200-mL beaker. Allow the mixture to stand for 24 hours at room temperature, shake frequently. 
Filter the solution to collect the precipitate, wash it with water to remove any ammonia, and boil with ethyl 



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Megalomania's Method of Making 2,4,6-Trinitro-<i>m</i>-Phenylenediamine 



alcohol to remove any non-reacted trinitro-m-anisidine or trinitro-m-phenetidine. You will need a graduated 
cylinder for measuring liquids, and a i rring or magnetic stirrei for mixing. 




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2004 



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Megalomania's Method of Making tetracene 




melting point 


boiling point 


tetracene 


molecular mass 


density 


explodes at 160 °C 


— 


188.76 g/mol 


0.45 g/mL 


table key 


sensitivity 

high 


chemical formula 
C 2 H 8 Ni 0 O 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





NH 

H N-( 

HN N-lf N-N-H 

^ / | \ 

/ N H NO 

H 2 N h 


(*> 





l-guanyl-4-nitrosoaminoguanyltetrazene, more conveniently called tetracene, was first prepared back 
in 1910 by two scientists named Hoffmann and Roth. It is a colorless pale yellow, fluffy material with 
slight hygroscopic properties. It is stable at normal temperatures when wet or dry, but decomposes in 
boiling water. Tetracene is sensitive to friction, shock, and flame. Its brisiance is greatest when it has not 
been compacted, so this compound can easily become dead-pressed. Tetracene is not suited for blasting 
caps or alone as an explosive since it does not detonate itself very efficiently. It is best suited for booster 
charges or in blasting caps mixed with other explosives. It can only achieve is full explosive potential if 
detonated by another explosive charge. The only problem I have noted with this lab is the 
aminoguanidine bicarbonate used as the main ingredient. I have found no literature whatsoever to 
suggest that this substance exists although it is probably a rare analog of aminoguanidine reacted with a 
bicarbonate substance, and given a non IUPAC name. 





CHEMICALS 


APPARATUS 1 


acetic acid 


3-liter Florence flask 1 




aminoguanidine bicarbonate 


graduated cylinder I 


sodium nitrite 


thermometer [ 





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Megalomania's Method of Making tetracene 



water 



Prepare a solution of 34 g of aminoguanidine bicarbonate and 12.5 mL of glacial acetic acid with 
2500 mL of watei in a 3 -liter Florence flask . Gently warm the flask on a steam bath and shake 
periodically until everything is completely dissolved into solution. The solution should be filtered to 
remove any impurities that may have not dissolved, then cooled to 30° C by running cold water from the 
faucet over the flask. It is necessary to filter the solution if there are impurities present. Add 27.6 g of 
sodium nitrite to the solution while swirling to dissolve it. Set the flask aside at room temperature for 3 
or 4 hours then shake it vigorously to start precipitation of the product. Let the flask stand for another 20 
hours. After standing, decant as much of the solution off as possible and drown the remaining crystals 
with water. Decant and drown with water several more times to wash the crystals. Filter the washed 
crystals to collect them and thoroughly wash again with water. Dry the product at room temperature and 
store in a sealed glass container to keep out the moisture. You will need a graduated cylinder for 
measuring liquids, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making TeNN 






melting point 
204 °C 


boiling point 
decomposes 


TeNN 


molecular mass 
308.16 g/mol 


density 
1.6 g/mL 




table key 


sensitivity 

low 


chemical formula 

c 10 h 4 n 4 o 8 


explosive velocity 
7013 m/s 


estimated cost 

$?.00/g 


A 










TeNN is an acronym for tetranitronaphthalene. There are actually several isomers of TeNN, we are 
primarily concerned with 1,3,6,8-tetranitronaphthalene as it forms in abundance over the 1,2, 4, 6-; 

1,2, 5, 8-; 1,2, 6, 8-; 1,3, 5, 7-; 1,3, 5, 8-; and 1,4,5,8-tetranitronaphthalenes. A mixture of isomers is bound to 
occur, though. TeNN is a very powerful and quite stable high explosive compound. It is actually slightly 
more powerful that TNT and just as stable. This explosive is superb because of its primary ingredient 
naphthalene. Naphthalene is the chemical name for moth balls, it is cheap, easy to get, not to hazardous, 
and sold in a store near you. I keep waiting for the government to ban it, or some environMeNtaList 
whacko to launch a save the moths campaign to ban it. The only drawback to TeNN is the possibility of 
side reactions reducing the yield during synthesis. Rapid heating of TeNN will cause it to explode, but 
slow heating will only cause decomposition. This lab uses concentrated sulfuric and nitric acids which 
are not so common, but still obtainable. Making TeNN is a multi step synthesis, first making mononitro 
then 1,8-dinitronaphthalene. 









CHEMICALS 


APPARATUS 




acetone 


1000-mL beaker 




ethyl alcohol 


2000-mL beaker 




naphthalene 


graduated cylinder 







http://www.roguesci.org/megalomania/explo/TeNN.html (1 of 3)12-8-2004 17:25:32 





Megalomania's Method of Making TeNN 



nitric acid 



potassium nitrate 



sulfuric acid 



water 



stirrer/stirring rod 



thermometer 



Prepare a mixture of 64 g of powdered naphthalene with 105 mL of water in a 1000-mL beaker . 
Slowly add 160 mL of 95% sul iric a to the beaker then add 81 mL of 70% nitric acid . Stir this 
mixture occasionally and allow it to cool to room temperature. During a 3 hour period, slowly add with 
stirring 150 g of powdered naphthalene to the acid mixture. The temperature will rise, regulate the 
addition of the naphthalene to get the temperature at 50 °C by the end of the addition time. After all of 
the naphthalene has been added, continue stirring and heat the beaker to 55 °C for several minutes then 
stop stirring and allow the mix to cool. Some mononitronaphthalene should crystallize on the surface of 
the beaker. 



Prepare a second nitrating mixture by putting 300 mL of 53% sulfuric acid in a 1000-mL beaker. 

Cool the acid to 25 °C by placing in a salt-ice bath. Add 152 g of potassium nitrate to the acid while 
stirring rapidly. Remove the mononitronaphthalene from the previous reaction and crush it up, add it in 
small bits while stirring to the mixture, maintain the temperature between 38 °C and 45 °C. The addition 
should require about 1 hour, do not allow the temperature to go over 45 °C at any time during the 
addition. After the addition, continue stirring and heat the beaker to 55 °C until the formation of 
dinitronaphthalene crystals begin. Filter the contents of the beaker on an acid filter to collect the crystals 
of dinitronaphthalene that should have formed. Wash the crystals with six portions of cold water and 
allow them to dry. Dissolve the dry crystals in boiling acetone . Filter this solution while hot to remove 
any undissolved impurities, collect the filtrate and allow it to cool by placing in a salt-ice bath. Filter to 
collect the pure crystals of dinitronaphthalene. Collect the acetone filtrate from this filtering, boil it to 
reduce the volume by half, and cool in a salt-ice bath. Again filter to collect a second crop of 
dinitronaphthalene, add these crystals to the previous and allow them to dry. 

Prepare the final nitrating acid mixture by slowly adding 750 mL of 100% sulfuric acid to 750 mL of 
100% fuming nitric acid in a 1000-mL beaker . Cool the acid mix to below 20 °C with a salt-ice bath. 
Once below this temperature, slowly add with stirring the dry dinitronaphthalene from the previous 
reaction while maintaining the temperature at 20 °C during the addition. After the addition, slowly heat 
the mixture to 80 °C over a 1 hour period ( 1 degree higher every minute) then hold the temperature at 80- 
90 °C for 3 hours more. Allow the mixture to cool then filter on an acid filter to collect the crystals of 
TeNN that should have formed. Collect the filtrate and drown it in ice water to precipitate additional 
crystals of TeNN. Filter to collect these crystals and combine them with the other crystals. Wash the 
crystals with several portions of water then add them to 95% ethyl alcohol . Allow the crystals to 
dissolve, then cool in a salt-ice bath to recrystallize the now pure TeNN. The pure crystals can be 
filtered to collect them and dried by heating on a steam bath. 



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Megalomania's Method of Making TeNN 



You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for 

mixing, and a thermometer to monitor the temperature for these procedures. 




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Megalomania's Method of Making TACC 




A 




melting point 


boiling point 


TACC 


molecular mass 
215.12 g/mol 


density 
? g/mL 


table key 


sensitivity 

high 


chemical formula 
[Cu(NH 3 ) 4 ]C10 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





o 



o' 



o 

A 

o 

II 

-CL 



'O' 



nh 2 

' 2+ 



H 2 N 

■O" 




A 



TACC is an acronym for tetraamminecopper (II) chlorate. It is a somewhat sensitive primary 
explosive compound, useful for detonators, but too dangerous for larger quantities. TACC is rendered 
useless by moisture and by being dead-pressed. TACC is safe to handle in the open, it can only be 
detonated while confined, otherwise it just burns with a green flame. In order for TACC to detonate in a 
blasting cap it must be filled as a loose powder then protected from moisture. The chemicals used in this 
preparation are not very common but can be obtained or synthesized. 





CHEMICALS 


APPARATUS 




ammonia 


bubbler 


cupric sulfate 


desiccator 


ethvl alcohol 


500-mL Erlenmever flask 


methvl alcohol 


evaporation dish 


sodium chlorate 


500-mL Florence flask 




graduated cylinder 



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Megalomania's Method of Making TACC 



magnetic stirrer 



Prepare a mixture of 15 g of sodium chlorate and 24 g of cupric sulfate in 360 mL of anhydrous ethyl 
alcohol in a round-bottomed -mL Florence flask . Anhydrous methyl alcohol can be substituted for 
ethyl alcohol. Reflux the contents of the flask for 30 minutes at the boiling point of the alcohol, or as 
close as can be reached depending on how efficient your reflux column is. You will need to stir the 
mixture with a magnetic stirrer during the reaction. After refluxing you should have a green solution. 
Filter this solution to remove any impurities that may remain. Add the filtrate to a 500-mL Erlenmeyer 
flask and bubble dry ammonia gas through the liquid for 20 minutes, the use of a bubbler can help. After 
this time the solution should be dark blue. After the ammonia addition, pour the liquid into an 
evaporation dish and allow it to evaporate to half its original volume. You can use a fan or low heat to 
speed up the process. Crystals of TACC should precipitate after several hours. Filter the liquid to collect 
the crystals and wash them with 50 mL of very cold methyl alcohol . Put the crystals in a desiccator for 
24 hours to dry them, then store in an airtight container to protect against moisture. You will need a 
graduated cylinder for measuring liquids. 




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Megalomania's Method of Making Silver Fulminate 




A 



melting point 


boiling point 


silver fulminate 


molecular mass 


density 


explodes at 170 °C 


— - 


149.89 g/mol 


? g/mL 


table key 


sensitivity 
very high 


chemical formula 
AgCNO 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



+ 




Ag + 



Silver fulminate is a very sensitive primary explosive compound. It is most often found in "bang 
snaps" and other novelty pyrotechnic objects. Only very tiny amounts of silver fulminate should be 
prepared at once, the weight of the crystals can cause them to self detonate. Silver fulminate was first 
prepared in 1800 by Edward Howard in his research project to prepare a large variety of fulminates. For 
200 years it has been only useful as a curiosity explosive in toys and tricks. 



A 



CHEMICALS 


APPARATUS 




ethyl alcohol 


100/500-mL beaker 




nitric acid 


graduated cylinder 




silver 


thermometer 






water 



Heat 8 mL of 70% nitric acid in a 100-mL beaker to 35-38 °C. Add 1 g of silver metal to the acid. 
While the silver is dissolving it will produce toxic nitrogen dioxide fumes, use a fume hood or get to a 
well ventilated area. Some heating may be required to get all of the silver to dissolve. Put 15 mL of 95% 
ethyl alcohol in a 500-mL beaker set into a salt-ice bath. After the silver has dissolved, slowly add the 
solution to the alcohol while keeping the temperature below 18 °C. More toxic nitrogen dioxide will be 
released. The reaction should require about 25-30 minutes to complete, after which 200 mL of cold 
water is added to precipitate the silver fulminate. Decant off as much of the liquid as possible then 
drown the crystals with water. Filter to collect the crystals and wash them with 30 mL of ethyl alcohol. 



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Megalomania's Method of Making Silver Fulminate 




kOHHI 



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Flour or starch can be added to the crystals before filtering to add some degree of stability. Store the 
silver fulminate away from sunlight as it can decompose. You will need a graduated cylinder for 
measuring liquids, and a hermometer to monitor the temperature. 



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Megalomania's Method of Making RDX 




melting point 


boiling point 


RDX 


molecular mass 


density 


205 °C 


— 


222.12 g/mol 


1.82 g/mL 


table kev 


sensitivity 

low 


chemical formula 

c 3 h 6 n 6 o 6 


explosive velocity 
8500 m/s 


estimated cost 

$?.00/g 



A 





no 2 

> 

_-N. ,N^ 

o 3 n ^ no 2 







RDX, or cyclonite, is a very insensitive high explosive compound. The actual chemical name is 
cyclotrimethylenetrinitramine, although the chemical names hexahydro-l,3,5-trinitro-l,3,5-triazine; 
Hexogen; trimethylenetrinitramine; sym-tn methyl enetri nitramine ;Hexolite; 1,3,5-trinitrohexahydro-p- 
triazine ; 1 , 3 ,5 -trinitrohexahy dro- s-triazine ; cy clotrimrthy lene-trinitramine ; 1 , 3 ,5 -triaza- 1,3,5- 
trinitrocyclohexane; trinitrohexahy drotriazine; and T 4 are also used. RDX itself stands for Royal 

Demolition eXplosive and comes from Great Britain, cyclonite is the American usage, Hexogen is for 
Germans, and T 4 is Italian. RDX is a very powerful military explosive that can be stored for long 
periods of time and handled safely. RDX is usually mixed with other explosives and plasticizers to make 
a variety of useful compositions for military and civilian use, C-4 and Semtex are two such compounds. 
It seems so much RDX is made that most scientific books give industrial schematics for thousands of 
pounds instead of lab preparations. The laboratory methods here are not as efficient as in industry, but 
are fine. The first method uses methenamine, or hexamethylenetetramine, which can be purchased as 
heating tablets or synthesized in the lab. The second makes use of acetic anhydride, forbidden by the 
DEA, but it can be synthesized as well. 





CHEMICALS 


APPARATUS 


acetic anhydride 


500-mL beaker 


acetone 


1000-mL beaker 



http://www.roguesci.org/megalomania/explo/RDX.html (1 of 3)12-8-2004 17:25:35 




Megalomania's Method of Making RDX 



ammonium nitrate 



methenamine 



nitric acid 



paraformaldehyde 



sodium bicarbonate 



water 



graduated cylinder 



stirrer/stirring rod 



thermometer 



Put 335 mL of 100% nitric acic in a 500-mL beaker, cool the acid to below 30 °C by setting the 
beaker in a salt-ice bath. The nitric acid must be as concentrated as possible, it must also be free of 
nitrogen oxides. Slowly add 75 g of methenamine in small portions to the acid while stirring. The 
temperature must be kept between 20 °C to 30 °C during the addition. Once all of the methenamine has 
dissolved, slowly heat it to 55 °C while stirring, hold it to between 50-55 °C for 5 minutes, keep stirring. 
Now cool the mix to 20 °C then let it sit for 15 minutes. After standing, it is gradually diluted with three 
or four times its volume of cool water , this should precipitate the RDX from solution. Depending on 
how the gods of chemistry feel about your reaction it may take from minutes to hours to fully precipitate 
all of the RDX. Decant most of the liquid then add 1 L of 5% sodium bicarbonate solution to neutralize 
the remaining acid. Filter the mixture to collect the crystals of RDX that should have formed. Wash 
them with cold water, then with hot 5% sodium bicarbonate solution, and again with water. The RDX 
can be dried at room temperature or in an oven. Further purification can be accomplished by 
recrystallizing from acetone . You will need a graduated cylinder for measuring liquids, a stirring rod or 
magnetic stirrer for mixing, and a thermometer to monitor the temperature. 

The second procedure is as follows: Place 260 mL acetic anhydride in a 1000-mL beaker and add 105 
g powdered ammonium nitrate while stirring. Heat the beaker to 90 °C and remove the source of heat. 
Very slowly add 38 g of paraformaldehyde to the beaker, this addition will release toxic and flammable 
fumes, use a fume hood or go to an open area. After the addition, add the contents of the beaker to twice 
its volume of cold water to precipitate crystals of RDX. Filter the solution to collect the crystals and 
wash them with cold water then boiling water. The RDX can be purified by dissolving in the minimum 
amount of acetone then diluting with cold water. Filter the crystals to collect them and allow to dry in 
the open air. 



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Megalomania's Method of Making RDX 




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Megalomania's Method of Making PVN 




PVN 




melting point 
ignites at 175 °C 


boiling point 
175 °C ignites 


PVN 


molecular mass 
(89.05) n g/mol 


density 
1.0 g/mL 


table key 


sensitivity 

medium 


chemical formula 
(C 2 H 3 N0 3 ) n 


explosive velocity 
5000 m/s 


estimated cost 

$?.00/g 






PVN stands for polyvinyl nitrate, which means that this explosive is a continually linked chain of 
vinyl nitrate over and over again. The material appears to be a white powder if the polymer has fewer 
links in the molecule and as tough white strands if there are many links in the molecule. PVN was first 
prepared in Germany in 1929 by G. Frank and H. Kruger by nitrating polyvinyl alcohol. This laboratory 
procedure comes from, I believe, two French scientists named Chedin and Tribot who experimented on 
method of PVN preparation after WWII. The densities of PVN can vary depending on the density of the 
starting polyvinyl alcohol and range from a low 0.3 g/mL to 1.5 g/mL and corresponding detonation 
velocities of 2030 m/s to 6560 m/s. Obviously it is better to have a higher density product. This product 
has found a niche in military applications mainly in propellents, but not so much in industrial 
applications. 



CHEMICALS 



APPARATUS 



acetic anhydride 



250-mL beaker 



ethyl alcohol 



graduated cylinder 



nitric acid 



stirrer/stirring rod 



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Megalomania's Method of Making PVN 



polyvinyl alcohol 



sodium bicarbonate 



water 



thermometer 



vacuum desiccator 



Over a period of 1 hour, very slowly add 5 g of finely pulverized lolyvinyl alcohol (containing 10% 
moisture) to 100 mL of 99-100 nitric acid in a 0-mL beaker . The beaker should be in a salt-ice bath to 
provide cooling during the addition. Maintain constant stirring and a temperature of -8 °C throughout the 
addition, and for an additional 2 hours after the addition. The resulting slurry is slowly drowned in an 
equal volume of ice water while vigorously stirring. Filter this to collect the white powder that should 
have formed, wash the powder with water until neutral to litmus, then put it in clean water for 12 hours. 
Repeat the washing and standing process using 95% ethyl alcohol , and again repeat the process with 
12% sodium bicarbonate solution. Finally, the powder is washed with water until neutral to litmus, dried 
in the open air, then in a vacuum desiccator . The yield is about 96%. You will need a graduated cylinder 
for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the 
temperature. 

It may be possible to increase the nitration yield by adding the polyvinyl alcohol to :etic anhydride 
first and using more nitric acid, the procedure is followed as above. 

Here are the formulas for WC846 and M9 propellants: 

82% PVN 57.75% PVN 

10.2% nitroglycerin 40.0% nitroglycerin 
0.7% dinitrotoluene 1.50% potassium nitrate 
6.1% dibutylphthalate 0.75% ethyl centralite 
1.0% diphenylamine 0.50% ethyl alcohol 

And, yes, M9 does add up to 100.5%, the alcohol is supposed to be just trace amounts, but is listed as 
0.5% for some reason. 




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Megalomania's Method of Making PVN 



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Megalomania's Method of Making Propylpicrate 




Propylpicrate 




melting point 
43 °C 


boiling point 

? °C 


propylpicrate 


molecular mass 
271.21 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
(0 2 N) 3 C 6 H 2 0CH 2 CH 2 CH 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





Propylpicrate is also given the names of propyl- [2, 4, 6-trinitro-phenyl] -ether and picricacidpropyl 
ether. This substance is a colorless crystalline material that is soluble in a large number of organic 
solvents. The preparation is nothing special and the explosive is about 68% as powerful as TNT. 







CHEMICALS 


APPARATUS 1 



benzene 



beaker 



hydrochloric acid 



petroleum ether 



picryl chloride 



potassium hydroxide 



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Megalomania's Method of Making Propylpicrate 



n-propyl alcohol 



Prepare a warm solution of picryl chloride dissolved in n-propyl alcohol in a small beaker . Add this 
solution to an ice-cold solution of potassium hydroxide in n-propyl alcohol in another beaker. The 
orange precipitate that should have formed is hydrolyzed with dilute hydrochloric acid to form a yellow 
solid. The crude propylpicrate is then dissolved in mzene and treated with decolorizing carbon. Final 
precipitation is then performed using petroleum ether . 




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Megalomania's Method of Making Potassium Picrate 




Potassium Picrate \! 






melting point 
explodes at 310 °C 


boiling point 


potassium picrate 


molecular mass 
267.20 g/mol 


density 
1.852 g/mL 


table kev 


sensitivity 

low 


chemical formula 
C 6 H 2 (N0 2 ) 3 0K 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 






A 



Potassium picrate was first prepared back in the mid 17th century by J.R. Glauber. The first use for 
potassium picrate came in 1869, it found its way into explosives, propellents, primers, and pyrotechnics. 
This explosive is stable and resists shock, friction, etc. It will deflagrate if subjected to flame, and in 
mixtures with oxidizing agents, it will only burn if ignited, but it has lower sensitivity. This is not a very 
powerful explosive, it is more suited to pyrotechnics and bullet primers. 











CHEMICALS 


APPARATUS 




nitric acid 


beaker 1 




picric acid 






potassium carbonate 






Potassium picrate can be prepared bv Glaubers original method of dissolving wood in nitric acic then 



neutralizing the resulting mixture with potassium carbonate . For the modern method, neutralize a hot 
aqueous solution of potassium carbonate with a hot picric acid solution in a beake: of suitable size, test 



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Megalomania's Method of Making Potassium Picrate 



the solution with litmus paper until neutral. Filter the crystals that separate when the solution cools to 
collect them and allow to dry. 




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Megalomania's Method of Making Nitrostarch 




Nitrostarch 




melting point 


boiling point 


nitrostarch 


molecular mass 
varies 


density 
0.88 g/cc 


table key 


sensitivity 

low 


chemical formula 
[C 6 H 7 (0H) x (0N0 2 ) y ] n 


explosive velocity 
4000-6000 m/s 


estimated cost 

$?.00/g 



X 

! 

W"/ ? x 



Y 



z 

unknown 




Nitrostarch, also called NS; nitrate d'amidon; nitrostaerke; and staerkenitrat, is actually a mixture of 
several nitrate esters of starch. Yes, starch is the plant product that can be purchased in the grocery store. 
Since this is really a variety of nitrated products the formula is [C5H 7 (0H) x (0N02) y ] n where x+y=3 and 
n is any whole number from one on up. The exact composition depends on the reaction conditions 
during the nitration. Nitrostarch found a use as a filler in hand grenades back in WWII, and also in 
mining explosives. Nitrostarch was first made when H. Barconnot nitrated cellulose and starch back in 
1833. At that time nitrocellulose and nitrostarch were thought to be one and the same. Then A. Bechamp 
applied various methods of separating them in 1862. The US first began to produce nitrostarch in 1888 
under the name Volney Powder. Various companies produced nitrostarch throughout both world wars, 
but the US emerged as its sole manufacturer. 



CHEMICALS 



APPARATUS 



nitric acid 



500-mL beaker 



sodium bicarbonate 



graduated cylinder 



starch 



stirrer/stirring rod 



sulfuric acid 



water 



thermometer 



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Megalomania's Method of Making Nitrostarch 



Prepare a mixture of 100 mL of 98-100% nitric acid and 138 mL of 95-100% sulfuric acid in a 500- 
ml beaker by pouring one acid into the other. Add the acids slowly as a lot of heat will be generated, 
keep the beaker in a salt-ice bath to cool it. Slowly add 100 g of starch to the acid mix while stirring and 
maintain a temperature of 10-12 °C for 1 hour and 50 minutes, continue stirring during the nitration. 

You can increase the rate of the reaction by holding the temperature to as much as 40 °C, but keep in 
mind higher temperatures increase the chance of accidents. Information on purifing and stabilizing the 
product is sketchy because of trade secrets, I suggest adding the nitrostarch to watei and bring it to a 
boil. Then add the nitrostarch to another batch of water in which a small amount of base has been added, 
like sodium bicarbonate , and bring to a boil. This should stabilize and purify the nitrostarch. The 
nitrostarch is then filtered to collect it and dried. You will need a graduated cylinder for measuring 
liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making Nitrosoguanidine 




A 




melting point 
explodes at 165 °C 


boiling point 


nitrosoguanidine 


molecular mass 
147.09 g/mol 


density 
? g/mL 


table key 


sensitivity 

high 


chemical formula 

c 2 h 5 n 5 o 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





A 




Nitrosoguanidine is technically called N-methyl-N'-nitro-N-nitrosoguanidine, other names include 
MNNG; N-methyl-N-nitroso-N'-nitroguanidine; N'-nitro-N-nitroso-N-methylguanidine; l-methyl-3- 
nitro-1 -nitrosoguanidine; methylnitronitrosoguanidine; N-nitroso-N-methylnitroguanidine; 1-methyl-l- 
nitroso-N-methylguanidine; 1-nitro-N-nitroso-N-methylguanidine; MNG; and methyl-N'-nitro-N- 
nitrosoguanidine. Nitrosoguanidine is a yellow, crystalline powder, it is a primary explosive that 
detonates producing little heat and no flash. Although this is a sensitive explosive, exploding from 
shock, friction, and elevated temperatures, it does not have powerful explosive properties and can be 
stored indefinitely if dry in a sealed bottle. This compound will slowly decompose in the presence of 
water and will explode on contact with sulfuric acid. I have instructions concerning a demonstration of 
its flashlessness in a darkened room involving placing 0.5 g on the back of the left hand. A match is lit 
and blown out, the heated match stick is touched to the powder and it explodes. Suffice to say DO NOT 
try this. The only after affects are a rash and peeling of the skin if you want to know... 



CHEMICALS 


APPARATUS 


ammonium chloride 


800-mL beaker 




nitro guanidine 


graduated cylinder 


water 


magnetic stirrer 


zinc 


thermometer 



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Megalomania's Method of Making Nitrosoguanidine 



Prepare a mixture of 21 g of nitro guanidine , 1 1 g of ammonium chloride , 18 g of zinc dust , and 250 
mL of water in an 800-mL beaker . Cool this mixture in a salt-ice bath and keep the temperature between 
20-25 °C while stirring with a magnetic stirrer . After 2 hours of stirring the gray color of the zinc should 
have disappeared and the mixture should now be yellowish, there should be no crystals floating around 
as well. Keep stirring a while longer if not. Next, cool the mixture to 0 °C or lower with the salt-ice bath. 
Filter the mixture to collect the nitrosoguanidine, discard the filtrate. The yellow residue of 
nitrosoguanidine will contain some zinc oxide or hydroxide and basic zinc chloride. The residue must be 
extracted with 4 successive portions of 250 mL of water heated to 65 °C. Combine the extracts and 
allow them to stand at 0 °C for 12-24 hours, nitrosoguanidine will precipitate out of the solution. Filter 
to collect the crystals, rinse them with water, and dry at 40 °C. Yield is about 8. 0-9. 2 g or 45-52% of the 
theoretical yield. You will need a graduated cylinder for measuring liquids, and a thermometer to 
monitor the temperature. 




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Megalomania's Method of Making 1,1,1,3,5,5,5-Heptanitropentane 




1 ,1 ,1 ,3,5,5,5-Heptanitropentane 




melting point 
decomposes at 104 °C 


boiling point 


1,1, 1,3, 5, 5, 5 -heptanitropentane 


molecular mass 
387.24 g/mol 


density 
1.74 g/cc 


table key 


sensitivity 

medium 


chemical formula 

(N0 2 ) 3 CCH 2 CH(N0 2 )CH 2 C(N0 2 )3 


explosive velocity 
? m/s 


estimated cost 
$?.00/g 




This explosive looks like white crystals, it is stable, able to resist heat and friction up to a point, and stores 
well for several weeks. What little data there is has been provided by L.T. Carleton from Aerojet Engineering Co. 
in 1951. 



CHEMICALS 


APPARATUS 


methvl alcohol 


beaker/ lask 


nitric acid 


desiccator 


nitroallyl acetate 


graduated cylinder 


sodium hydroxide 


pipet/buret 


trinitromethane 


stirrer/stirring rod 


water 


thermometer 



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Megalomania's Method of Making 1,1,1,3,5,5,5-Heptanitropentane 



Prepare a solution of 7.5 g of nitroallyl acetate and 20 mL of methyl alcohol in a beaker or Erlenmeyer flask , 

and cool. Slowly add the cold solution drop by drop, with a dropper pipe or auret , to a constantly stirred mixture 
of 15.1 g of rinitromethane in 150 mL of water maintained at 0 °C over a period of 1 hour. Add 1 mL of a 20% 
solution of odium hydroxide to the mixture of trinitrome thane and water before the acetate and alcohol addition. 
The hydroxide will act as a catalyst for the reaction. The product is washed with water and recrystallized from 
70% ntrie acid at 75 °C. The product is then dried in a iesiccator . Yield is about 66%. You will need a graduated 
cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the 
temperature. 




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Megalomania's Method of Making Hexamethylenetetramine Dinitrate 




Hexamethylenetetramine Dinitrate 






melting point 
165 °C (dec) 


boiling point 


hexamethylenetetramine dinitrate 


molecular mass 
266.21 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 

c 6 h 14 n 6 o 6 


explosive velocity 
6000 m/s 


estimated cost 

$?.00/g 







N+NCy 

NOf 


f§> 







Hexamethylenetetramine dinitrate, also called HDN, is a rather weak high explosive made from a 
quite simple reaction between methenamine and a nitrating mixture forming a quaternary ammonium 
salt. It is fairly stable to heat, shock, and friction but it is somewhat hygroscopic. This explosive is a 
close cousin to the far superior RDX, but HDN does not really stand out as anything exceptional from a 
military perspective. The reaction is quite simple and straightforward for the improvisational chemist. 
Two different methods of preparation are presented here and the molar ratios may be scaled up or down 
as required. 



A 



CHEMICALS 


APPARATUS 




acetone 


250-mL beaker 


ammonium nitrate 


desiccator 


hydrochloric acid 


graduated cylinder 




methenamine 


stirrer/stirring rod 


nitric acid 


thermometer 






water 



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Megalomania's Method of Making Hexamethylenetetramine Dinitrate 



Dissolve 14 g (0.1 mol) of methenamine in 50 mL of warm water in a 250-mL beaker . Place the 
beaker of solution into a salt-ice bath and cool it to 5 °C or less. Measure out 20 mL (0.314 mol) of 70% 
nitric acid into a small test-tube or beaker and cool the acid in the ice bath as well. It is not necessary to 
use 70% acid as long as the proper molar amount is added, just limit the amount of water the 
methenamine is dissolved in accordingly if dilute acid is used. Slowly add the nitric acid, with stirring, 
to the methenamine solution at such a rate as to keep the temperature below 5 °C. The addition of the 
acid should cause the immediate precipitation of product. Continue stirring a minute after all of the acid 
has been added to insure complete precipitation, and then pour the mixture over a vacuum filter to 
collect the crystals. Hexamethylenetetramine dinitrate can be decomposed by water into formaldehyde in 
short order, so no extra time should be taken. Wash the crystals with several portions of dry icetone or 
anhydrous ethyl alcohol to remove any last trace of acid and to accelerate drying. Place the crystals in a 
desiccator to dry. Store in a tightly closed vial to protect from moisture. You will need a graduated 
cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to 
monitor the temperature. 

An alternative to using nitric acid in this synthesis is to use a nitrate salt and hydrochloric acid. The 
yields may be a bit less, but the result is the same. Instead of preparing a hexamine solution, prepare a 
nitrating solution by dissolving 28 g (0.35 mol) of ammonium nitrate in 80 mL (0.8 mol) of 31.45% 
hydrochloric acit in a 250-mL beaker. Cool this solution in a salt-ice bath to 0 degrees. Again, it is not 
necessary to use the specified concentration of hydrochloric acid as long as the proper molar amount is 
added. Dissolve 14 g (0.1 mol) of methenamine in a minimum amount of water (about 21 mL). Quickly 
add this solution to the nitrating mix with rapid stirring; a precipitate should soon form. Filter and wash 
the crystals as above. One could substitute sodium nitrate or potassium nitrate of the same molar mass in 
place of ammonium nitrate. 




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January 31, 2004 



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Megalomania's Method of Making Hexanitrocarbanilide 




melting point 
decomposes at 208 °C 


boiling point 
explodes at 345 °C 


hexanitrocarbanilide 


molecular mass 
? g/mol 


density 
? g/mL 


table key 


sensitivity 

medium 


chemical formula 

C 6 H 2 (N0 2 ) 3 NHC0NHC 6 H 2 (N0 2 )3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



r'VKT (> 


no 2 o 2 n 

— / o 

'A II // 


\\ 




) In L/ jn t 

/ H H \ 


IN KJ 2 




\ / 
no 2 o 2 n 





This particular explosive is of curious interest, it is not really used that much but it still explodes. It is a pale yellow 
crystalline substance that melts with some decomposition at 208 °C. It is very brisant, usually used in detonators or 
booster charges. The explosive force is slightly greater than TNT. The primary ingredient is carbanilide, also known as 
sym-diphenylurea, which can be made from heating aniline and urea together at 160-165 °C, or by the interaction of 
phosgene and aniline. A more technical name for this explosive is 2,2',4,4',6,6'-hexanitro-N,N'-diphenylurea or sym- 
dipicrylurea. 









CHEMICALS 


APPARATUS 


carbanilide 


beaker 


nitric acid 


buret/separatory funnel 


sulfuric acid 


Erlenmeyer flask 


water 


Florence flask 




graduated cylinder 


stirrer 


thermometer 



40 g of carbanilide is dissolved in 60 mL of 100% sulfuric acic in a small beaker , pour the solution into a buret or 
separatory funnel and add it drop by drop during a 4 hour period in to 96 mL of 100% nitric acid , in an Erlenmeyer 
flask , while the mixture is stirred vigorously with a mechanical stirrer and its temperature is maintained at 35° to 40° C. 



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Megalomania's Method of Making Hexanitrocarbanilide 



After all of the solution has been added, the stirring is continued and the temperature is raised to 60 °C over 30 minutes 
and held at that temperature for another 60 minutes. The mixture is allowed to stand over night where it can cool to 
room temperature. After sitting, crushed ice and water are added to the solution, then it is poured over a filter to collect 
the crystals that should have formed. The crude tetranitrocarbanilide is washed thoroughly with water and allowed to 
dry in the air. In the second stage, 10 g of crude tetranitrocarbanilide is added to a mixture of 9 mL of concentrated 
sulfuric acid and 16 mL of nitric acid in a small dorencc flask , and the material is heated on a steam bath or hotplate, 
to no more than 100 °C, for 1 hour with constant stirring. After cooling, crushed ice and water are added to the mixture, 
then it is poured over a filter to collect the crystals. The product is washed with 500 mL of cold water, then treated with 
500 mL of hot water, and dried in the air. The resulting hexanitrocarbanilide is of good quality for use as an explosive. 
You will need a graduated cylinder for measuring liquids, and a r hermometer to monitor the temperature. 




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Megalomania's Controversial Chem Lab ©1997-2004 /hexanitrocarbanilide/ revised June 14, 2004 



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Megalomania's Method of Making Hexanitrodiphenylamine 




Hexanitrodiphenylamine 




A 




melting point 
decomposes at 243 °C 


boiling point 


hexanitrodiphenylamine 


molecular mass 
439.22 g/mol 


density 
1.58 g/mL 


table key 


sensitivity 

low 


chemical formula 
(C 6 H 2 (N0 2 ) 3 ) 2 NH 


explosive velocity 
6900 m/s 


estimated cost 

$?.00/g 






2,2',4,4',6,6'-hexanitrodiphenylamine, also known as dipicrylamine, hexamine, hexamin, heksyl, 
hexil, hexamite, hexite, or usually hexyl, was first prepared back in 1874 and was used as early as 1910 
in both world wars, mostly by the Germans. Other scientific names include 2,4,6-trinitro-N-(2,4,6- 
trinitrophenyl)- benzenamine; 2,4,6-Trinitro-N-(2,4,6-trinitrophenyl)benzenamine; and Bis(2,4,6- 
trinitrophenyl)amine. Foreign names include esanitrodifenilammina o exil in Italian; 
hexanitrodifenilamina o hexamina in Spanish; and gheksonitrodifenilamin in Russian. 

Hexyl forms yellow needles in its crystalline state and decomposes slightly at its melting point of 243- 
245 °C. Hexyl is slightly hygroscopic at room temperature so keep it stored tightly away from air. Hexyl 
is very toxic, attacking the skin and causing severe burns. It causes respiratory irritation of the nose and 
throat if inhaled. Hexyl is not really a sensitive compound, it can be heated up to 250 °C before 
detonating if heated at a rate of 5 °C a minute. It can be detonated by severe shock, but you would have 
to treat it pretty badly. Drop tests caused detonations when a 2 kg weight fell from 60 cm. The explosive 
power is around 6900 m/s and increases with greater density to around 7150 m/s at 1.67 g/cc which is 
comparable to TNT. 

The Germans and the Japanese used this explosive in admixture with TNT in torpedoes, sea mines, 
depth charges, and bombs. Commercially this explosive was used in compositions called Neurodits. The 
Swedish used it in compositions called Novit. The Germans mixed it with aluminum powder in 
compositions called Schieewolle 18, and it was also used in German skip bombs. The Japanese used it in 
compositions called Seigata (aka Type 97), and Otsu-B. 



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Megalomania's Method of Making Hexanitrodiphenylamine 





CHEMICALS 


APPARATUS 




acetone 


500-mL beaker 




aniline 


graduated cylinder 




calcium carbonate 


pipet/buret 


dinitrochlorobenzene 


stirrer/stirring rod 






hydrochloric acid 


thermometer 






nitric acid 


petroleum ether 


sulfuric acid 


water 



Synthesis 1: 

This preparation will be carried out in two stages forming dinitrophenylamine, tetranitrophenylamine, 
and finally hexanitrodiphenylamine. 70 mL of aniline and 32 g of pure calcium carbonate are stirred up 
together with 300 mL of vate: in a 500-mL beaker to form a homogeneous suspension, and the mixture 
is heated to about 60 °C. 150 g of previously melted dinitrochlorobenzene is slowly added by pouring in 
a fine stream from a beaker while the stirring is continued and the mixture is gradually heated to about 
90 °C, the rate of heating being regulated by the progress of the reaction which can be determined by the 
formation of dinitrophenylamine. The product is poured over a filter to collect the crystals, washed with 
hydrochloric acid to free it from aniline and calcium carbonate, then with water until free from 
chlorides, and dried in an oven at 100 °C. 

In the first stage, 50 g of finely powdered dinitrodiphenylamine (formed from the above process) is 
added in small portions to 315 mL of 50-55% nitric acid in a 500-mL beaker, which is stirred vigorously 
while the temperature is maintained at 50-60 °C. The progress of the nitration is followed by observing 
the color change from the red of the dinitro compound to the yellow of the tetranitrodiphenylamine. 

After the dinitrodiphenylamine has been added, the temperature is raised to 80-90 °C and kept there for 
two hours longer while the stirring is continued. After the mixture has cooled, the product is filtered off 
directly, washed with water until free from acid, and dried in the air or in an oven at 100 °C. 

In the second stage, 50 g of tetranitrodiphenylamine (formed in the first stage) is added slowly from 
a ripet or buret , with stirring, over one hour, to a mixture of 170 mL of 100% nitric acid and 140 mL of 
100% sulfuric acid in a 500-mL beaker. After all of the tetranitrodiphenylamine has been added, the 
mixture is allowed to stand for 3 hours at room temperature, and is then drowned in ice water. The 



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Megalomania's Method of Making Hexanitrodiphenylamine 



hexanitrodiphenylamine that should have formed is filtered off, washed thoroughly with water, dried in 
the air, and recrystallized from acetone with the addition of petroleum ether . You will need a graduated 

cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to 

monitor the temperature. 

Synthesis 2: 

Into a 1000-mL Florence flask containing 500 mL of concentrated sulfuric acid (100%) slowly add, 
while swirling the flask, 50 g of roughly ground diphenylamine. Into a 5-L round-bottomed flask 
immersed in an ice bath place 333 mL (500 g) of fuming nitric acid (100% with 5-10% dissolved 
nitrogen dioxide). Set the flask up for addition and slowly add the sulfuric acid solution drop by drop to 
the nitric acid while maintaining a temperature of 30 C. After adding all of the solution heat the flask on 
a steam bath until no more nitrogen dioxide gas escapes (CAUTION: this gas is toxic, use adequate 
ventilation!). The blue colored solution should fade and yellow crystals will precipitate. Allow the 
mixture to cool to room temperature and then slowly pour it into a large container of 5 L of ice water. 
Pour this solution over a filter to collect the product and wash it thoroughly first with cold and then with 
hot water until no trace of acid remains. Dry the product in an oven at 100 C. Yield is about 88 g. The 
product may be purified by recrystallization from 75% nitric acid. 




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Megalomania's Controversial Chem Lab ©1997-2004 /hexanitrodiphenylamine/ revised June 23, 2004 



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Megalomania's Method of Making Dinitrochlorobenzene 






melting point 
52-54 °C 


boiling point 
315 °C 


dinitrochlorobenzene 


molecular mass 
202.55 g/mol 


density 
1.7 g/mL 


table key 


sensitivity 

low 


chemical formula 
C 6 H 3 C1(N0 2 ) 2 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





Cl 



- n °2 



Cl 



major 



N0 2 



N0 2 no 2 



© 



minor 



During the early chemical industry days of World War I there was a lot of spare chlorine floating 
about and there was a big demand for benzene which made it cheap and available. Put em together and 
you get chlorobenzene and dichlorobenzene, of which p-dichlorobenzene is a type of mothball still used 
today. The nitration of chlorobenzene was started around 1862 by A. Riche. Dinitrodichlorobenzene was 
first manufactured as an explosive called parazol. It was mixed with with TNT in shells but did not 
detonate completely. Instead, the unexploded portion was atomized in the air and was a vigorous itch- 
producer and lachrymator (causes tears like mace), it also yielded some phosgene gas which was a 
dreadful chemical weapon used back then. Dinitrochlorobenzene finds more use as an ingredient in the 
manufacture of other explosives than as an actual explosive itself, although it has been mixed with picric 
acid for use in shells. Avoid contact with the solid and vapors of this chemical, it causes severe itching, 
as well as weakness, low blood count, digestive organ damage, and heart failure. The proper name of 
this compound is l-chloro-2, 4-dinitrobenzene for the most abundant isomer, and 2-chloro- 1,3- 
dinitrobenzene for the other isomer. Other names include 2,4-dinitro-l -chlorobenzene; 2,4- 
dinitrochlorobenzene; l,3-dinitro-4-chlorobenzene; chlorodinitrobenzene; DNCB; and 4-chloro- 1,3- 
dinitrobenzene. 



CHEMICALS 



APPARATUS 



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Megalomania's Method of Making Dinitrochlorobenzene 



chlorobenzene 


1000-mL beaker 




nitric acid 


graduated cylinder 


sulfuric acid 


pipet/buret 


water 


stirrer/stirring rod 


thermometer 



90 mL of chlorobenzene is added dropwise with a dropper )ipet or buret to a previously prepared, 
and cooled to room temperature, mixture of 1 10 mL of 99% nitric acid and 185 mL of 99% sulfuric acid , 
in a lOOO-mL beakei , while the mixture is stirred mechanically with a magnetic stirrer . A stirrer is 
essential for the length of time required, you may try this by hand with a stirring rod at your own risk. 
The temperature will rise because of the heat of the reaction, but should not be allowed to go above 50- 
55 °C. After all the chlorobenzene has been added, the temperature is slowly raised to 95 °C and is kept 
there for 2 hours longer while the stirring is continued. An upper layer of light yellow liquid solidifies 
when cold. The layer is removed, broken up under water , and rinsed. The spent acid, on dilution with 
water, will precipitate an additional quantity of dinitrochlorobenzene. All the product is brought 
together, washed with cold water, then several times with hot water while it is melted, and once more 
with cold water under which it is crushed. Finally, it is drained and allowed to dry at room temperature. 
The product, melting at about 50 °C, consists largely of 2,4-dinitrochlorobenzene, along with a small 
quantity of the 2,6-dinitro compound, m.p. 87-88 °C. The two substances are equally suitable for 
manufacture of other explosives or alone as an explosive. You will need a graduated cylinder for 
measuring liquids, and a hermometer to monitor the temperature. 




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Megalomania's Method of Making Dinitropolystyrene 






melting point 
260 °C 


boiling point 

? °C 


dinitropolystyrene 


molecular mass 
>38000 g/mol 


density 
0.25 g/mL 


table key 


sensitivity 

low 


chemical formula 
[C 6 H 3 (NO 2 ) 2 (CHCH 2 )] 200 


explosive velocity 
1510 m/s 


estimated cost 

$?.00/g 






Dinitropolystyrene, or nitropolystyrene, is a very interesting explosive procedure involving the 
nitration of everyday polystyrene. That's the same stuff as Styrofoam, all those containers from fast food 
restaurants and packing from boxes. This lab calls for isotactic polystyrene, which is the crystalline 
version. I suppose you can use ordinary Styrofoam. This material has found a home as a mining 
explosive since it is stable and somewhat low powered. It will burn in the open and requires a suitably 
powerful explosive plus confinement to detonate. 





CHEMICALS 


APPARATUS 


nitric acid 


small beaker 


polystyrene 


stirring rod 


fuming sulfuric acid 




water 





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Megalomania's Method of Making Dinitropolystyrene 



Dinitropolystyrene is prepared by nitrating isotactic, or crystalline, polystyrene. Prepare an anhydrous 
nitration mixture by bubbling sulfur trioxide into concentrated sulfuric acid, making fuming sulfuric acid 
with about 50% free sulfur trioxide. Mix this acid with 100% nitric acid in the ratio of 4.51 parts nitric to 
2 parts sulfuric in a small beaker . An example would be 45. 1 mL of nitric acid mixed with 20 mL of 
sulfuric acid. Add the acids slowly and cool the mixture to 15-20 °C. While maintaining the cool 
temperature, add in the crystalline polystyrene . If you are using foamed polystyrene, break it up as much 
as possible. Add only as much as can still be covered by the acid. Stir the polystyrene for 3-5 minutes 
with a stirring rod , then heat the mixture to 50-55 °C for 2 hours, stirring occasionally. Next, cool the 
mixture down to 25 °C and decant off as much of the acid as possible. Drown the dinitropolystyrene 
with water to dilute the remaining acids. Pour the contents over a filter to collect the dinitropolystyrene, 
wash it several times with water, and allow to dry. The yield should be about 33%. One explosive 
mixture uses 7.2% dinitropolystyrene along with 10.8% dinitrotoluene and 82.0% PETN. The detonation 
velocity of this mixture is 7520 m/s. 




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Megalomania's Method of Making Dinitrobenzene 




Dinitrobenzene 




melting point 


boiling point 


dinitrobenzene 


molecular mass 


density 


kO 

o 

0 

n 


291 °C 


168.11 g/mol 


1.5751 g/mL 


table key 


sensitivity 

low 


chemical formula 
C 6 H 4 (N0 2 ) 2 


explosive velocity 
6100 m/s 


estimated cost 

$?.00/g 







Dinitrobenzene comes in three isomers, they are ortho, meta, and para-dinitrobenzene. The most 
important explosive isomer is meta-dinitrobenzene, or just m-dinitrobenzene, other names include 
dinitrobenzol; 1,3 -dinitrobenzene; 2,4-dinitrobenzene; binitrobenzene; and 1,3-dinitrobenzol. This 
material was used as a replacement for TNT back in World War I since it was somewhat more 
economical. The Russians used dinitrobenzene from 1914 to 1918 as a filling for naval mines, in 
Germany it was called Di-Fiillpulver, DiFp for short, for use in shells. An earlier explosive called 
Hellhoffites mixed nitric acid and dinitrobenzene, this was used in 1897-1880. This compound was first 
prepared by St. C. Deville in 1841 by treating benzene with concentrated nitric acid and boiling. I should 
warn you that this particular substance is very toxic, poisoning may be caused by inhaling the vapors or 
by absorption through the skin. The volatility is rather low but a concentration as low as 1 mg per cubic 
meter of air can cause acute poisoning. Poisoning is more likely in warm weather when the vapor 
pressure is higher due to the increased temperature. So keep it cool, don’t touch it and wear some sort of 
respirator. Frequent exposure and past poisoning will increase the probability of future poisoning. 
Women, especially, should stay away as it affects them more than men. The sensitivity of m- 
dinitrobenzene is quite low, it requires an initiator charge to detonate it. This procedure requires 
nitrobenzene as the main ingredient, the preparation of which is in the synthesis section. This procedure 
makes about 92% meta, and an 8% mix of ortho and para isomers. 



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Megalomania's Method of Making Dinitrobenzene 



CHEMICALS 


APPARATUS 


ethyl alcohol 


Erlenmeyer flask 


nitric acid 


graduated cylinder 


nitrobenzene 


pH paper 


sodium hydrogen sulphite 


stirring rod 




sodium hydroxide 


thermometer 


sulfuric acid 




water 





To prepare dinitrobenzene, heat a mixture of 14 mL of concentrated ;ulfuric acid and 10 mL of 
concentrated nitric acic in an open Erlenmeyer flash in a boiling water bath in an area with good 
ventilation. 10 g of litrobenzene is added gradually over a period of 30 minutes. The mixture is allowed 
to cool somewhat, then drowned in cold water . The dinitrobenzene should separate as a solid. Crush it 
under water with a stirrii | rod , wash with water, and recrystallize from ethyl alcohol or nitric acid. 
Dinitrobenzene crystallizes from nitric acid in beautiful needles which are practically colorless. Further 
purification by removing the ortho and para isomers can be achieved by reacting the product with 
sodium sulphite, it is not necessary to do this, but it will give a highly refined product. The 
dinitrobenzene is added to a 33% sodium hydroxide solution and heated to 50 °C while vigerously 
stirring. The temperature must be monitored with a thermometer to insure it does not rise above 80-85 ° 
C. The total washing time is 30 minutes. During the washing, the pH must be alkaline, test often with pH 
paper. If at any point the pH is not alkaline, add more sodium hydroxide solution. Next, sulphitation of 
dinitrobenzene is done by adding cold water to the above alkaline solution until the temperature falls to 
66 °C. Then, a solution of sodium sulfite, prepared by mixing a 40% solution of sodium hydrogen 
sulphite with half its volume of 33% sodium hydroxide solution, is added. Maintain the temperature at 
66-73 °C while stirring for 2 hours. Afterwards, cool the mix to 50 °C and the purified dinitrobenzene 
will precipitate into large crystals. The majority of the liquor can be decanted off and the crystals poured 
over a filter to collect them. Wash the crystals throughly by repeated rinsings with water. The final 
product can be dried at 135 °C under reduced pressure. You will need a graduated cylinder for 
measuring liquids. 



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Megalomania's Method of Making Dinitrobenzene 




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Megalomania's Controversial Chem Lab ©1997-2004 /dinitrobenzene/ revised January 31, 2004 



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Megalomania's Method of Making DDNP 




melting point 


boiling point 


DDNP 


molecular mass 


density 


? °C 


? °C 


? g/mol 


1.63 g/mL 


table key 


sensitivity 

high 


chemical formula 

c 6 h 2 n 4 o 5 


explosive velocity 
6900 m/s 


estimated cost 

$?.00/g 



A 



A 




G-N 

0 2 N^^L^N 

no 2 











DDNP is an acronym for diazodinitrophenol, it is also known as 4,6-dinitrobenzene-2-diazo-l -oxide, 
and Dinol. DDNP is a picric acid derivative with somewhat good stability and explosive velocity. It is 
still susceptible to heat, friction, and shock making it a primary explosive. Its preparation is very simple, 
needing only picramic acid, sodium or potassium nitrite, and some dilute hydrochloric or sulfuric acid. 
Obtaining the picramic acid will be impossible for most, so I included how it can be prepared in the 
synthesis section. This compound was first prepared by Dr. Griess in 1858, this led him to conduct 
ground breaking research on the diazotization reaction. 





CHEMICALS 


APPARATUS 




acetone 


250-mL beaker 




hydrochloric acid 


graduated cylinder 




picramic acid 


magnetic stirrer/stirring rod 


sodium nitrite 


thermometer 


water 





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Megalomania's Method of Making DDNP 



Diazodinitrophenol is prepared by a diazotization reaction, this happens when an amine substituient, 




NH 2 , on an aromatic ring, , loses its hydrogen atoms and forms a triple bond with another 

nitrogen atom. Place 120 mL of 5% hydrochloric acid in a 250-mL beaker , then immerse the beaker in a 
salt-ice bath. Place the ice bath on top of a magnetic stirrer and drop a spin bar in the beaker. Slowly add 
10 g of picramic acid to the acid solution while stirring rapidly, monitor the temperature with a 
thermometer . Be sure there is no sudden rise in temperature. If you do not have a magnetic stirrer, use a 
stirring rod and stir like the wind. Dissolve 3.6 g of sodium nitrite in 10 mL of water . After the picramic 
acid has dissolved, add the sodium nitrite solution all at once and continue stirring for 20 minutes. Filter 
the solution to collect the dark brown crystals that should have formed and wash them with cold water. 
The diazodinitrophenol thus formed can be used as is, or it can be purified by dissolving in hot acetone 
then precipitated by adding a large volume of ice water while rapidly mixing the liquid. This treatment 
will convert the diazodinitrophenol into bright yellow crystals. You will need a graduated cylinder for 
measuring liquids. 

The diazodinitrophenol must be dried before it will explode. Drying will take 24 hours if done at 
room temperature, or in 2 hours if the crystals are placed in a beaker suspended in hot water. The 
diazodinitrophenol must be stored in a sealed glass container. Storing the explosive moist, about 25% 
water, will increase safety. Dry immediately before use. DDNP will detonate if it is struck by a sharp 
blow, but it will only burn rapidly if ignited in the open, even several grams. 




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Megalomania's Method of Making DADNPE 






melting point 


boiling point 


DADNPE 


molecular mass 


density 




64 °C 


135 °C decomposes 


276.24 g/mol 


? g/mL 




table key 


sensitivity 


chemical formula 


explosive velocity 


estimated cost 




very high 


c 5 h 8 n 8 o 6 


? m/s 


$?.00/g 


A 











The name of this explosive is 3,3-diazido-2,4-dinitratopentane, and that is about all I know for this 
compound except it is very sensitive to friction and shock. It has been proposed as a propellant and as a 
percussion primer for caseless ammunition. 





CHEMICALS 


APPARATUS 




acetic anhydride 


dropper pipet 


3,3-diazido-2,4-pentanediol 


Erlenmeyer flask 




ethyl ether 


graduated cylinder 


hexane 


magnetic stirrer 


nitric acid 


thermometer 


water 



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Megalomania's Method of Making DADNPE 



Prepare a nitrating solution by slowly adding 4.56 mL of 100% nitric acid with a dropper pipet to 
10.68 mL of rcetic anhydride in a small Erlenmeyer flask , and cool the solution to 0-5 °C. While 
maintaining the temperature at 5-15 °C, add 4.2 g of solid 3,3-diazido-2,4-pentanediol over a period of 
20 minutes. Stir the mixture for 30 minutes, with a magnetic stirrer or by occasionally swirling the flask, 
after which time some crystallization should have occurred. Complete precipitation is achieved by 
drowning the mixture in an excess of ice water . The product is extracted with ethyl ether and 
recrystallized from lexane. The yield is about 85%. You will need a graduated cylinder for measuring 
liquids and a thermometer to monitor the temperature. 




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Megalomania's Controversial Chem Lab ©1997-2004 /DADNPE/ revised January 31, 2004 

The Preparation of Some New Polyfunctional Organic Azides 



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Megalomania's Method of Making DADNBU 








melting point 
70 °C 


boiling point 
150 °C decomposes 


DADNBU 


molecular mass 
262.21 g/mol 


density 
? g/mL 


table key 


sensitivity 
very high 


chemical formula 
(N0 3 )CH 2 CHN 3 CHN 3 CH 2 (N0 3 ) 


explosive velocity 
? m/s 


estimated cost 1 

$?.00/g 


■ 




A 



The name of this explosive is 2,3-diazido-l,4-dinitratobutane. All I know about this compound, other than 
how to synthesize it, is that it is very sensitive to friction and shock. It has been proposed as a military 
propellant. 





CHEMICALS 


APPARATUS 


acetic anhydride 


Erlenmeyer flask 


2,3-diazido- 1 ,4-butanediol 


graduated cylinder 


ethyl alcohol 


dropper pipet 


nitric acid 


magnetic stirrer 


thermometer 



Prepare a 1 to 1 molar solution of nitrating acid by slowly mixing 12.3 mL of acetic anhydride and 5.5 mL 
of 100% nitric acid in a small Erlenmeyer flask. Cool the solution to 0-5 °C in a salt-ice bath. Slowly add 



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Megalomania's Method of Making DADNBU 



2.58 g of 2,3-diazido- 1 ,4-butanedio drop by drop with a pet to the cool acid. Add the diol at such a rate 
that the reaction temperature stays between 5-15 °C. Stir the mixture during the addition and for 30 minutes 
afterwards with a magnetic stirrer or by swirling the flask. Several recrystallizations from ethyl alcohol give 
fairly pure product with an approximate yield of 40%. You will need a graduated cylinder for measuring 
liquids and a hermometer to monitor the temperature. 




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Megalomania's Controversial Chem Lab ©1997-2004 /DADNBU/ revised January 31, 2004 

The Preparation of Some New Poly functional Organic Azides 



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Megalomania's Method of Making <font face="Symbol">a</font>-Benzenediazobenzyl Hydroperoxide 




a-Benzenediazobenzyl Hydroperoxide 




A 




melting point 
65 °C decomposes 


boiling point 


a-benzenediazobenzyl 

hydroperoxide 


molecular mass 
228.28 g/mol 


density 
? g/mL 


table key 


sensitivity 
very high 


chemical formula 
C 6 H 5 N=NCH(OOH)C 6 H 5 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





A 




This compound has the appearance of canary yellow needles. I have very little information about this 
compound other than it is sensitive to light, it may explode on standing, it is insensitive to friction or 
impact, but will explode on contact with flame, concentrated sulfuric acid, and nitric acid. This 
explosive was first prepared around 1914. 





CHEMICALS 


APPARATUS 




benzaldehvde phenvlhvdrazone 


bubbler 




benzene 


Erlenmever flask 




oxygen 


graduated cylinder 


petroleum ether 





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Megalomania's Method of Making <font face="Symbol">a</font>-Benzenediazobenzyl Hydroperoxide 



Prepare a mixture of 1 g of benzaldehyde phenylhydrazone suspended in 6 mL of benzene in a small 
Erlenmeyer flask . Y ou can make any volume desired, but keep the same 1 g per 6 mL ratio, keep in 
mind the danger increases in making more. While constantly shaking the mixture, bubble oxygen gas 
through it for 6 hours. It may seem bothersome to shake this stuff all the time and I doubt you have an 
automatic shaker, so you might be able to get away with shaking it for a minute every 10 to 15 minutes. 
Inserting the end of some rubber tubing from your oxygen generator may not yield good results, it is far 
better to use a bubbler similar to a fish tank aerator. A bubbler may be somewhat costly, but better in the 
long run, you can use a fish tank aerator but it may dissolve in the benzene (this has happened to me, the 
aerators are just sand pressed together). Another potential problem is that there will not be enough room 
for a fish tank aerator , with such a low volume of solution since they are cylindrical, whereas bubblers 
can be flat. After the oxygen addition, add cold )etroleum ether to crystallize the product out of solution. 
Pour the crystals over a vacuum filter to collect and dry them faster. The yield is about 73%. Keep the 
product away from light and dispose immediately as it may detonate on standing. You will need a 
graduated cylinder to measure liquids. 




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Megalomania's Controversial Chem Lab ©1997-2004 /a-benzenediazobenzyl hydroperoxide/ revised 
January 31, 2004 

Organic Peroxides 



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Megalomania's Method of Making Benzalaminoguanidine Nitrate 




Benzalaminoguanidine Nitrate 




melting point 
160.5 °C 


boiling point 

? °C 


benzalaminoguanidine nitrate 


molecular mass 
? g/mol 


density 
? g/mL 


table key 


sensitivity 


chemical formula 


explosive velocity 


estimated cost 


unknown 


C 6 H 5 CH=NHNHC(NH)NH 2 no 3 h 


? m/s 


$?.00/g 



A 




I don't have much information on this explosive other than it is a derivative of the explosive 
nitroguanidine as it uses that material as its precursor. I would assume it has properties similar to 
nitroguanidine. This explosive may also be called benzaldehyde guanylhydrazone nitrate. 



A 



CHEMICALS 


APPARATUS 


acetic acid 


Erlenmeyer flask 


benzaldehyde 


small beaker 




ethyl alcohol 


graduated cylinder 




nitric acid 


stirring rod 



nitroguanidine 


thermometer 


water 




zinc dust 





Into a 300-mL Erlenmeyer flask , add 26 g of zinc dust , 10.4 g of nitroguanidine , and 150 mL of 



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Megalomania's Method of Making Benzalaminoguanidine Nitrate 



water . Slowly add 42 mL of glacial acetic acid from a small beaker at such a rate that the temperature of 
the mixture does not rise above 40 °C. The liquid at first turns yellow because of the formation of 
nitrosoguanidine but becomes colorless again when the reduction is complete. After all the zinc has 
disappeared, add 45 mL of concentrated nitric acid , then 102 mL of benzaldehyde . Shake the mixture 
well to mix the contents then scratch the inside of the flask with a glass stirring roc to facilitate the 
precipitation of benzalaminoguanidine nitrate crystals. The product can be purified by recrystallizing 
from water or from ethyl alcohol . You will need a graduated cylinder for measuring liquids and a 
thermometer to monitor the temperature. 




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Megalomania's Controversial Chem Lab ©1997-2004 /benzalaminoguanidine nitrate/ revised January 
31,2004 

The Chemistry of Powder and Explosives 



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Megalomania's Method of Making Astrolite 




melting point 


boiling point 


Astrolite 


molecular mass 


density 


? °C 


? °C 


— 


? g/mL 


table key 


sensitivity 
very low 


chemical formula 


explosive velocity 
8600 m/s 


estimated cost 

$?.00/g 



A 





X 

W"/ ? x 

z 1 

unknown 


C‘> 





Astrolite is not a chemical compound but rather a two component high explosive mixture. Its claim to 
fame is it has the highest explosive velocity of all chemical explosives, a distant second only to a nuclear 
blast, a claim that is entirely false. Only that anarchist crap still thinks that Astrolite is super powerful. 
The truth is, its low density makes it unlikely to achieve a detonation comparable to more common 
explosives Astrolite G is a mixture of ammonium nitrate and hydrazine, Astrolite A adds aluminum 
powder to the mix for extra power. Hydrazine is a very toxic, corrosive, and dangerous chemical that 
you will never be able to get. The fumes can kill you in seconds if breathed in a confined area. I have 
devoted a section to hydrazine and its safety in the chemical synthesis section. 





CHEMICALS 


APPARATUS 


aluminum powder 


beaker 


ammonium nitrate 


graduated cylinder 


hvdrazine 


stirring rod 





To make Astrolite G, add 200 g of ammonium nitrate to a large beaker and stir in 100 mL of 
hydrazine , mix well. For Astrolite A add 40 g of aluminum powder to the Astrolite G mixture. It is best 
to make the mixture immediately before use because the ammonium nitrate becomes sensitive to 
detonation once hydrazine is added. Professional blasters make their mixtures in the field at the blast site 



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Megalomania's Method of Making Astrolite 



for greater safety. Each component is measured out in separate containers, transported to the site, mixed, 
allowed to sit for 20 minutes, and detonated. As separate components they are very safe (well as safe as 
hydrazine can get) and the mixing is easy. Astrolite can be detonated even when it has been poured out 
on the ground and left for 4 days. More Astrolite can be prepared by observing a 2:1 ratio of ammonium 
nitrate to hydrazine by weight and 1:5 of aluminum powder to ammonium nitrate by weight. You will 
need a graduated cylinder for measuring liquids and a stirring rod for mixing. 




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Megalomania's Method of Making HMTD 




A 




melting point 
decomposes at 75 °C 


boiling point 


HMTD 


molecular mass 
? g/mol 


density 
0.88 g/mL 


table key 


sensitivity 
very high 


chemical formula 
N(CH 2 -0-0-CH 2 ) 3 N 


explosive velocity 
4511 m/s 


estimated cost 

$?.00/g 











/:h 2 -o-ch 2v 

n-ch 2 -o-ch 2 -n 

"CH 2 -0— CH / 


(•> 







HMTD, or hexamethylenetriperoxidediamine, is a somewhat unstable primary explosive compound. 
Its extreme sensitivity to heat, shock, and friction make HMTD a poor choice for the lesser skilled home 
chemist. This lab uses hydrogen peroxide at 30% concentration, it is possible to use the more common 
3% concentration by adding ten times as much. The hexamethylenetetramine used here, also called 
hexamine, methenamine, or urintropine, can be purchased as "heating tablets." As to what heating tablets 
are... They are used in camping and in the military for heating meals, or hand warmers. It is very 
unlikely that you will find this anymore, so synthesize your own as described in the chemical synthesis 
section. HMTD has been used as a detonator, it is safer and more powerful than mercury fulminate or 
acetone peroxide. It is stable when compared to other primary explosives, and it is one of the safest 
explosive peroxides. HMTD should be kept cool and dry as it may evaporate or decompose, it should 
also be kept away from metals as it will corrode them. HMTD will detonate if struck, but will only burn 
if heated. 





CHEMICALS 


APPARATUS 


citric acid 


200-mL beaker 




methenamine 


graduated cylinder 




hydrogen peroxide 


stirrer/stirring rod 








methyl/ethyl alcohol 


thermometer 


water 





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Megalomania's Method of Making HMTD 



Dissolve 14 g of methenamine in 50 mL of 30% hydrogen peroxide in a 200-mL beaker while 
stirring vigorously with a magnetic stirrer or with a stirring rod . Y ou must also cool this solution by 
placing the beaker in a salt-ice bath. While stirring, slowly add 21 g of powdered citric acid in small 
portions to the beaker making sure the temperature stays at or below 0 °C at all times. After adding the 
citric acid, keep stirring for 3 hours and continue to hold the temperature at 0 °C. Next, remove the 
beaker from the cooling bath and let it stand at room temperature for 2 hours, discontinue stirring as 
well. Finally, pour the solution over a filter to collect the crystals of HMTD, wash them thoroughly with 
water , and rinse with metfn or eth\ alcohol so they can dry faster at room temperature. Dry by setting 
in a cool place. HMTD does not store well, so deal with it immediately. You will need a graduated 
cylinder for measuring liquids, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making HMX 




HMX 






melting point 
281 °C 


boiling point 

? °C 


HMX 


molecular mass 
296.16 g/mol 


density 
1.903 g/mL 




table key 


sensitivity 
very low 


chemical formula 

c 4 h 8 n 8 o 8 


explosive velocity 
91 10 m/s 


estimated cost 

$?.00/g 


A 











HMX is a very powerful military explosive with similar properties to RDX, the other great military 
explosive with which it is often mixed. HMX is technically called octahydro-1, 3,5,' 7-tetranitro-l, 3,5,7- 
tetrazocine, other names include 1,3, 5,' 7-tetranitro-l, 3, 5,' 7-tetrazacyclooctane; cyclotetramethylene 
tetranitramine; and octogen. HMX is itself an acronym for either High velocity Military eXplosive, or 
Her Majesties eXplosive depending on what country you are in. HMX is very stable, it requires a 
powerful detonator or booster charge to detonate. It was first developed during WWII in the never 
ending search for more powerful bombs. 



CHEMICALS 



APPARATUS 



acetic acid 



500/1000-mL beaker 



acetic anhydride 



500-mL Florence flask 



ammonium nitrate 



graduated cylinder 



methenamine 



stirrer/stirring rod 



nitric acid 



thermometer 



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Megalomania's Method of Making HMX 



paraformaldehyde 

water 



Prepare a solution of 748 mL of glacial acetic acid , 12 mL of acetic anhydride , and 17 g of 
paraformaldehyde , keep this solution at 44 °C while mixing. Prepare a second solution of 217.6 g of 
ammonium nitrate and 154.6 mL of 99% nitric acid in a 500-mL beaker . Prepare a third solution of 101 
g of methenamine , 157 mL of glacial acetic acid, and 296 mL of acetic anhydride in a 1000-mL beaker. 
Combine the third solution with 112.5 mL of the second solution. Add this combined solution to the first 
solution over a 15 minute period while stirring rapidly. After the addition, continue stirring for an 
additional 15 minutes. Next, carefully add 296 mL of acetic anhydride, then carefully add the remainder 
of the second solution, then add another 148 mL of acetic anhydride, all while stirring. Continue the 
stirring for 1 hour more. After stirring, add 350 mL of hot water and reflux the whole works for 30 
minutes. After this time, cool the liquid down to 20 °C by adding ice. Decant off as much of the liquid 
from the precipitate as possible and drown the remaining crystals with cold water. Filter to collect the 
crystals of HMX and wash them with three portions of cold water, allow to dry. The yield is about 95%. 
You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, 
and a hermometer to monitor the temperature. 

Owing to the large volume of reactants in this lab, in excess of 2.5 L, it is necessary to use a 5-L 
flask, unfortunately this is beyond most laboratories, and especially the home chemist. This reaction can 
be carried out in a glass gallon jug or similar large capacity glass container. The refluxing step can be 
done in portions using a round-bottomed )00-niL Florence flask . 




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Megalomania's Method of Making HNIW 




A 



melting point 


boiling point 


HNIW 


molecular mass 


density 


decomposes at 260 °C 


— 


438.19 g/mol 


1.98 g/mL 


table kev 


sensitivity 
very low 


chemical formula 
C 6 H 6 N 12°12 


explosive velocity 
10300 m/s 


estimated cost 

$?.00/g 



A 





HNIW is an acronym for hexanitrohexaazaisowurtzitane, other names include CL- 20; octahydro- 
l,3,4,7,8,10-hexanitro-5,2,6-(iminomethenimino)-lH-imidazo[4,5-b]pyrazine; 2,4,6,8,10,12-hexanitro- 
2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0 5 ’ 9 .0 3 ’ 11 ]dodecane; and 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12- 
hexaazaisowurtzitane. HNIW is a new kid on the block, it was first prepared by A.T. Nielsen in 1987, 
and has since been proposed as a propellent for bullets and as a blasting explosive. There are actually 6 
crystalline isomers of HNIW, this lab will prepare the beta form, although some of the alpha form will 
probably be made. The other isomers are made by heating the crystals to its decomposition point, the 
alpha and beta forms are the most stable. This explosive will most likely be the standard workhorse of 
the 21st century, it is currently still in testing for useful applications. HNIW is a symmetric 
polyazacyclic nitramine, itself a type of caged polynitramine, a promising new series of compounds. 
HNIW is similar to RDX and HMX in structure and explosive properties. This is a two part lab, the first 
synthesizing a derivative called tetraacetyldibenzylhexaazaisowurtzitane (TADB), then from that, 
HNIW. 





CHEMICALS 


APPARATUS 






acetic anhydride 


500-mL Florence flask 






bromobenzene 


graduated cylinder 


chloroform 


stirrer/stirring rod 



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Megalomania's Method of Making HNIW 



N,N-dimethylformamide 



thermometer 



ethyl acetate 



ethyl alcohol 



HBIW 



hydrogen 



nitrogen 



nitrosyl tetrafluoroborate 



Pearlman's catalyst 



sulfolane 



water 



Prepare a solution of 129 mL of N,N-dimethylformamide and 65 mL of acetic anhydride in a round- 
bottomed 00-mL Florence flask . Add to the flask, with stirring, 43.2 g of , 0.8 mL of 
bromobenzene , and 4.7 g of Pearlman’s catalyst . Purge the flask by bubbling hydrogen gas in the liquid , 
this will displace the air. Continue to bubble hydrogen gas into the flask and stir. If possible, maintain a 
pressure of 50 psi. Over a short period of time, the temperature may rise to about 50 °C, at this 
temperature begin cooling the flask with a cold water or salt-ice bath to keep it under 50 °C. The total 
reaction time needed is 24 hours. Since it is undesirable to bubble hydrogen gas through the flask for this 
length of time, as much would be wasted, a pressure is maintained. During the reaction, stop cooling if 
the temperature drops below 35 °C, always keep it between 35-50 °C. Stir the contents of the flask for 
the entire 24 hours. Purge the flask by bubbling nitrogen gas into it to displace any remaining hydrogen. 
Filter the contents of the flask to collect the solid material and the catalyst. Wash with 130 mL of 
denatured ethyl alcohol , this should leave behind a gray solid of Pearlman's catalyst and TADB. The 
TADB can be separated from the catalyst by dissolving the solid in boiling chloroform , and filtering to 
remove the remaining solid catalyst. Boil the chloroform down to recrystallize the TADB. The yield is 
about 85%. 



Prepare a solution of 15.5 g of the above prepared TADB, 1.1 mL of watei, and 300 mL of sulfolane 
in a round bottomed 500-mL Florence flask on a salt-ice bath. Add 10.5 g of nitrosyl tetrafluoroborate to 
the flask over a period of 30 minutes, keeping the temperature below 25 °C. After the addition, stir the 
mixture for 1 hour at 25 °C, then for 1 hour at 55-60 °C. Allow the solution, which should be a yellow- 
orange color, to cool to 25 °C. After cooling, rapidly add 47.8 g of nitrosyl tetrafluoroborate, keeping the 
temperature below 25 °C. Stir the mixture at 25 °C for 2 hours, then at 55-60 °C for 2 hours. Cool the 
mixture to below 10 °C with a salt-ice bath, then dump the contents, solid precipitate and all, into a large 
bucket. Slowly add 4.5 L of water to the mixture in the bucket, keeping the temperature below 25 °C, the 



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Megalomania's Method of Making HNIW 



color of the solution should change from green to yellow, some brown fumes may be evolved. Maintain 
the temperature at 25 °C with continuous stirring for 18 hours, a white precipitate should form. Filter to 
collect this crude HNIW, and wash several times with water to yield about 12 g of hydrated product. To 
purify the HNIW, dissolve it in 40 mL of ethyl acetate , chromatographically filter the solution through a 
short column of silica get, and wash with ethyl acetate. Pour the filtered solution into 500 mL of 
chloroform to precipitate the HNIW in its anhydrous beta form. The chromatographic filtration can be 
skipped. If pale yellow crystals are obtained as the crude product, it is the wrong stuff. Heat these 
crystals in 15 mL of water per 1 g of product at 95 °C with stirring for 10 minutes, then cool to 0 °C. 
After standing for 6 hours, filter and wash the crude product as above, it should be HNIW now. You will 
need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a 
thermometer to monitor the temperature. 




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Megalomania's Method of Making HNO 




melting point 


boiling point 


HNO 


molecular mass 


density 


? °C 


? °C 


? g/mol 


? g/mL 


table key 


sensitivity 

low 


chemical formula 
(C 6 H 2 (N0 2 ) 3 NHC0) 2 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



A 





0 0 
c? v b 

OiN NH NH NCb 

\ / \ / 

— NO 2 0 2 N 

/ ^ 

N0 2 







HNO stands for 2,4,6,2',4',6'-hexanitro-oxanilide. This material uses the explosive TNO as its 
precursor. HNO was first prepared by A.G. Perkins in 1892 when he did nitrations of TNO and from 
oxanilide. HNO is a stable compound that resists mechanical shock, friction, and heat. Compared to 
TNO this compound is fairly similar, it has, perhaps, slightly greater stability and explosive power. HNO 
is used as a component in ignitors and pyrotechnics. 



CHEMICALS 



acetone 



ethyl alcohol 



nitric acid 



sulfuric acid 



tetranitro-oxanilide 



APPARATUS 



beaker 



Buchner funnel 



1000-mL Florence flask 



graduated cylinder 



litmus paper 






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Megalomania's Method of Making HNO 



water 


stirrer/stirring rod 




thermometer 



Prepare an acid mixture by pouring 125 mL of 90% nitric acid into a round bottomed )Q0-mL 
Florence flask . Slowly add 55 mL of concentrated sulfuric acid . Set the flask into a salt-ice bath and cool 
it to 10 °C. You will need a magnetic stirrer if using a flask, otherwise stir by hand with a stirring rod in 
a beakei with extreme caution. Slowly add 29.2 of tetranitro-oxanilide (TNO) to the mixed acid with 
rapid agitation while keeping the temperature between 8-10 °C, this should require about 25 minutes. 
After adding the TNO, transfer the flask to a water bath and heat it to 85 °C over a 2 hour period, then 
hold the temperature between 85-90 ° for 1 hour more. The HNO slurry is filtered on a Buchner funnel 
and washed with water until it is almost acid free. The filter cake is placed in a beaker and sufficient 
water added to form a slurry. Steam is run into the slurry under agitation for 10 minutes. The slurry is 
filtered and the residue washed. The latter treatment of the slurry is repeated until the wash water is 
found to be neutral to litmus paper . The HNO is washed with ethyl alcohol , then acetone , dried in the 
air, and finally dried at 100-110 °C. You will need a graduated cylinder for measuring liquids, and a 
thermometer to monitor the temperature. 




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Megalomania's Method of Making IPN 




4 



melting point 
-82 °C 


boiling point 
101.5 °C 


IPN 


molecular mass 
105.09 g/mol 


density 
1.036 g/mL 


table key 


sensitivity 

low 


chemical formula 
CH 3 CH(0N0 2 )CH 3 


explosive velocity 
5070 m/s 


estimated cost 

$?.00/g 



A 









\ 

p 


:i 

+ ... 









IPN is an acronym for isopropyl nitrate, its proper scientific name is 2-propyl nitrate. IPN is a white 
liquid with an ether like smell. IPN is a volatile liquid with anesthetic properties at lower concentrations 
as well as causing headaches if inhaled or spilled on the skin. Ingesting or constant inhalation of 
quantities exceeding 4% for two or more hours is lethal. Quantities as low as 0.2% show no ill effects. 
This substance has found uses as rocket propellents and jet starter fuel when it is not being used as a 
propellent or explosive. The liquid is stable for the most part although it is flammable. 









CHEMICALS 


APPARATUS 




isopropyl alcohol 


Florence flask 1 




nitric acid 






urea 






To prepare IPN, isopropyl alcohol is nitrated continuously by adding a mixture of 61% nitric acid 



with 95% isopropyl alcohol , saturated with urea , into a Florence flask set up for distillation containing 



boiling 50% nitric acid. The IPN and water formed are continuously distilled off at about 98 °C from the 
reaction mixture. The volume of the reaction mixture is held constant by drainage of nitric acid and 
unstable by-products from it as the reactants are added. Unless you have a special flask with a stopcock 
on the bottom, you will have to periodically disconnect the flask from the condenser and dump out some 
of the used nitric acid. You will also have to momentarily disconnect the flask to add more acid/alcohol 
mix if you do not have an addition funnel. Be very careful doing this as you will subject yourself to a 



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Megalomania's Method of Making IPN 



blast of acid fumes. A curtain of air, nitrogen, or carbon dioxide is blown through the reaction mixture to 
improve mixing and to facilitate the elimination of the volatile products. However, a flow of inert gas in 
excess of 50 L/hr decreases the IPN yield. The optimum ratio of nitric acid to isopropyl alcohol is about 
2:1. The IPN yield is 78%. 




A jf\ La * 3 


Homel Explosivesl Chemical 


Weaponsl Pharmaceuticalsl Pesticidesl Precursors 


imer 


Skillsl Lab Eaui 


pmentl Safetvl Roque Sciencel Linksl What's New| Contact MelDisda 


Megalomanir 


t's Controversial Chem Lab ©1997-2004 /IPN/ revised January 31, 200 z 


1 





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Megalomania's Method of Making Lead Azide 




A 




melting point 
explodes at 350 °C 


boiling point 


Lead Azide 


molecular mass 
291.24 g/mol 


density 
3.8 g/mL 


table key 


sensitivity 

high 


chemical formula 
Pb(N 3 ) 2 


explosive velocity 
4500 m/s 


estimated cost 

$?.00/g 







n=n=n 

^n=n=n 







Lead azide is a common primary explosive used as a standard to compare sensitivity among other 
primary explosives. Making lead azide is not a simple task, this laboratory uses advanced techniques and 
equipment. Getting the chemicals will be another task. Sodium azide is an unstable, therefore regulated, 
material nearly impossible to get, it will need to be synthesized. Lead azide is sensitive to heat, shock 
and friction. The addition of dextrin to this lab prevents the formation of large crystals which can be 
very dangerous. 





CHEMICALS 


APPARATUS 


dextrin 


250-mL beaker 


lead nitrate 


Buchner funnel 


sodium azide 


graduated cylinder 




sodium hydroxide 


pipet/buret 


water 


separatory funnel 




stirring rod 




thermometer 



Dissolve 2.33 g of sodium azide and 0.058 g of sodium hydroxide in 70 mL of water by shaking in a 
separatory funnel . This is solution A. Dissolve 6.9 g of ead nitrate and 0.35 g of dextrin in 90 mL water 



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Megalomania's Method of Making Lead Azide 



in a 0-niL beaker , add 1 or 2 drops of 10% sodium hydroxide to bring the pH to about 5. This is 
solution B. Heat solution B to 60-65° on a water bath and agitate it with a plastic or hardwood stirring 
rod . The stirring should be as efficient as possible to prevent the formation of large crystals. Stirring, 
while vigorous, should not produce any spattering of the mixture and the stirring should not rub against 
the walls of the beaker. The friction might cause some crystals to explode. Add solution A dropwise to 
solution B while stirring. The addition should take about 10 minutes. Remove the beaker from the water 
bath and continue stirring the mixture in the beaker while cooling to room temperature, this will take 
about 1 hour. Allow the precipitate of lead azide to settle and pour the solution over a filter to collect the 
crystals. Use suction filtration with a Buchner funnel if possible. Add 150 mL of water to the crystals to 
wash them, add the water in 50 mL increments. Dry the sample for 8-15 hours or longer, but no more 
than 24, at 65 °C. The lead azide should form small spherical crystals that are opaque in color. The yield 
should be around 5 g. Store the lead azide moist in a rubber stoppered plastic bottle if you must. If you 
do not have a separatory funnel for solution A, use a beaker to prepare the solution and a pipet or buret 
to to add it to solution B. You will need a graduated cylinder for measuring liquids, and a thermometer 
to monitor the temperature. 




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Megalomania's Method of Making Lead Nitratophosphite 




Lead Nitratophosphite 




melting point 
decomposes at 100 °C 


boiling point 


lead nitratophosphite 


molecular mass 
668.43 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
Pb(N0 3 ) 2 Pb(H 2 P0 2 ) 2 


explosive velocity 
4500 m/s 


estimated cost 

$?.00/g 





Lead nitratophosphite, or LNP, is a stable heavy, white crystalline compound first prepared back in 
1916 by E.R. Von Hertz. This compound is not all that well suited as a stand alone explosive because of 
its high stability and small volume of gas produced. On the plus side, it makes an excellent component 
in mixtures and is practically smokeless, leaving little residue or slag. This compound is best suited for 
percussion fuses as it burns very hot in the open. 



CHEMICALS 



APPARATUS 



calcium hypophosphite 



beaker 



lead nitrate 



stirrer/stirring rod 



water 



Prepare a saturated lead nitrate solution by adding 331 g of it to 260 mL of hot water in a beaker . 
Prepare a saturated calcium hypophosphite solution by adding 170 g of it to 1360 mL of water, bring this 
solution to a boil. Add the hot lead nitrate solution slowly to the boiling calcium hypophosphite solution. 



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Megalomania's Method of Making Lead Nitratophosphite 



The mixture is then cooled rapidly, with efficient stirring, by placing it in a salt-ice bath upon which lead 
hypophosphite separates. Pour the solution over a filter to collect the lead hypophosphite. Add 250 g of 
the lead hypophosphite to a boiling solution of 500 g of lead nitrate in 1500 mL of water in a beaker 
while stirring, and cool rapidly. The LNP precipitate that should have formed is filtered and dried at 40- 
50 °C. You will need a stirring rod or magnetic stirrer for mixing. 




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Megalomania's Method of Making Lead Picrate 




A 




melting point 
explodes at 270 °C 


boiling point 


Lead Picrate 


molecular mass 
663.41 g/mol 


density 
2.831 g/mL 


table kev 


sensitivity 
very high 


chemical formula 
Pb(C 6 H 2 (N0 2 ) 3 0) 2 H 2 0 


explosive velocity 
4400 m/s 


estimated cost 

$?.00/g 





A 





Lead picrate is a very unstable primary explosive compound. Its manufacture is simple, and the 
chemicals used in the preparation are not all that exotic. The main ingredient in lead picrate is the 
explosive picric acid, its manufacture is listed in its own section. Another chemical precursor, lead 
monoxide, also known as litharge or white lead, is supposedly available for use in plumbing. If my 
plumber used lead in my pipes he would get fired. Check out plumbing stores but do not hold your 
breath. Until I actually find some for sale it would seem better to make it. Lead picrate crystals are very 
sensitive to friction, shock, and heat. The crystals may even detonate from their own weight. This 
explosive is usually found in a monohydrate form. It was first patented in France in 1872 for use in 
blasting caps and bullet primers. 





CHEMICALS 


APPARATUS 


lead monoxide 


small beaker 


methvl alcohol 


crystallization dish 


picric acid 


stirring rod 




graduated cylinder 



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Megalomania's Method of Making Lead Picrate 



In a small beaker , dissolve 2 g of picric acid in 10 mL of methyl alcohol and stir with a wooden or 
plastic stirring rod until the picric acid dissolves. Slowly add 2 g of ead monoxide to the solution while 
stirring. The solution may thicken at this time, you must prevent the formation of large clumps in 
solution or dried crystals on the side of the beaker. At this point pour the solution onto a crystallization 
dish and let it evaporate. The lead picrate can be dried faster by heating on a steam or water bath, this 
will give the product more stability as well. Dried lead picrate is very sensitive to friction, shock, and 
heat. A large pile of the crystals may detonate themselves from their own weight, so spread them out as 
much as possible. You will need a graduated cylinder for measuring liquids. 




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Megalomania's Method of Making Lead Styphnate 






melting point 
explodes at 275 °C 


boiling point 


lead styphnate 


molecular mass 
? g/mol 


density 
2.6 g/mL 


table key 


sensitivity 

high 


chemical formula 
PbC 6 H(N0 2 ) 3 0 2 


explosive velocity 
4900 m/s 


estimated cost 

$?.00/g 






A 



Lead styphnate, also called lead trinitroresorcinate, is an unstable primary explosive that resists shock 
but will detonate readily from heat or static. It is usually mixed with lead azide to improve its ability to 
detonate from flame or electric ignition. The preparation of lead styphnate is easy, but the chemicals 
used in its manufacture are of the kind only a lab would use. Lead acetate and nitric acid can be obtained 
but magnesium styphnate will be nearly impossible. Magnesium styphnate is derived from styphnic acid, 
or 2,4,6-trinitroresorcinol. Trinitro anything usually raises some danger flags, and dangerous chemicals 
are forbidden. Until I locate the method of preparation for styphnic acid, you will have to find some 
yourself. 



A 



CHEMICALS 


APPARATUS 


lead acetate 


small beaker 


magnesium styphnate 


graduated cylinder 


nitric acid 


stirring rod 




water 


thermometer 



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Megalomania's Method of Making Lead Styphnate 



Lead styphnate is prepared by adding a magnesium styphnate solution to lead acetate solution in a 
small beaker while stirring, and keeping the temperature at 70 °C. A precipitate will form, keep stirring 
for 15 minutes. After this time is up, add dilute nitric acid while stirring and cooling to 30 °C with a salt- 
ice bath, keep stirring until this temperature is reached. Collect the crystals on filter paper, wash with 
water , and allow them to dry in the open. The crystals should be reddish brown or orange in color. 

Notice the lack of quantities of chemicals. The source I obtained this information from is reliable but 
sketchy. I suggest using 10 g of lead acetate in 30 mL of water, and the same for magnesium styphnate, 
to make the solutions. Add 10 mL of concentrated nitric acid to 70 mL of water for the dilute acid. Keep 
in mind the danger these crystals may pose, keep the dried crystals away from heat, friction, and shock. 
Store the crystals under water if they are not going to be used immediately. You will need a graduated 
cylinder for measuring liquids, a stirring rod for mixing, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making Lead 2,4,6-Trinitro-3-Oxybenzoate 




Lead 2,4,6-T rinitro-3-Oxybenzoate 




A 



melting point 


boiling point 


lead 2,4,6-trinitro- 


molecular mass 


density 


— 


— 


3-oxybenzoate 


? g/mol 


? g/mL 


table key 


sensitivity 

medium 


chemical formula 
??? 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



A 




unknown 



This substance was first prepared by H. Ficheroulle and A. Kovache in 1949. This explosive is 
somewhat stable to mechanical shock but will explode when brought into contact with flame. The solid 
will pull moisture out of the air, being hygroscopic. The more moisture it contains, the less likely it is to 
explode, conversely the drier it is the more likely it is to explode. Keep this material tightly stoppered 
and perhaps damp when storing, but keep it dry for detonating. Thus far there have been no practical 
military or civilian applications for this compound. 



A 



CHEMICALS 


APPARATUS 


ethyl alcohol 


beaker 




lead nitrate 


graduated cylinder 




sodium benzoate 


stirring rod 




water 


thermometer 





Dissolve 2.4 g of lead nitrate in 50 mL of water heated to 90-95 °C in a beaker , and add, with stirring, 
a concentrated solution of sodium benzoate , prepared by neutralizing 2 g of benzoic acid with 0.6 g of 
sodium hydroxide. Evaporate the mixture on a water bath to a small volume while the liquid still 
remains clear. Cool and add 50 mL of 95% ethyl alcoho . This results in a very fine, light yellow 



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Megalomania's Method of Making Lead 2,4,6-Trinitro-3-Oxybenzoate 



precipitate, which is separated by vacuum filtration. After drying at 50 °C, the yield should be about 
41.82%. A moisture content in excess of 20% will make this explosive nearly impossible to detonate. 
You will need a graduated cylinder for measuring liquids, a stirring rod for mixing, and a thermometer 
to monitor the temperature. 








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,6-trinitro-3-oxybenzoate/ revised 



January 31, 2004 



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Megalomania's Method of Making Maltose Octanitrate 






melting point 
135 °C 


boiling point 
decomposes at 171 °C 


maltose octanitrate 


molecular mass 
702.30 g/mol 


density 
1.62 g/mL 


table key 


sensitivity 

high 


chemical formula 
Ci 2 Hi 4 0 3 (0N0 2 ) 8 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







Maltose octanitrate, also called nitromaltose, is a powerful, somewhat sensitive explosive used 
militarily in blasting caps. This compound does decompose over time, losing about 23% over a 43 day 
period, so it is best to use this compound within a reasonable time after preparation. In the mean time 
keep it stored in a cool place as elevated temperatures will accelerate the decomposition. A useful 
detonator called maltobenzit can be made by thoroughly blending 10 g of maltose octanitrate with 5 g of 
ra-dinitrobenzene at 70 ° in a kneading machine with 20 g of benzene. The resulting plastic mass is 
heated to 95 °C while the kneading is continued, and then cooled. 





CHEMICALS 


APPARATUS 


ethyl alcohol 


250-mL beaker/ lask 




ethyl ether 


graduated cylinder 


maltose 


pipet/buret 


nitric acid 


stirrer/stirring rod 



sodium bicarbonate 



thermometer 



sulfuric acid 



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Megalomania's Method of Making Maltose Octanitrate 



urea nitrate 
water 



Dehydrate 20 g of pure maltose by heating in a hot oven for 45-60 minutes. Throughly mix the dried 
maltose with 0.5 g of urea nitrate in a 250-mL beaker or Florence flask . Place the beaker or flask in a 
salt-ice bath and slowly add 40 mL of 99% nitric acid drop by drop with a pipe! or buret . Stir the 
mixture constantly during the acid addition and maintain a temperature of 0-2 °C. The liquid should turn 
a brownish color at this point. While stirring, slowly add 55 mL of fuming sulfuric acic containing about 
25% S0 3 . If at any point brown fumes begin to evolve, stop adding the acid and let it cool before 
continuing. After all the acid has been added, the mixture is warmed to 80 °C and poured into a large 
volume of ice water . The yellow solid precipitate that should have formed is seperated by filtration and 
washed sequentially with 1% sodium bicarbonate solution and water. To remove any remaining urea 
nitrate, the precipitate is recrystallized twice from a 1:2 ethyl alcohol / ethyl ether solution and dried. The 
yield should be a whopping 159% of the theoritical yield, or 31.8 g. You will need a graduated cylinder 
for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the 
temperature. 




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Megalomania's Method of Making Mannitol Hexanitrate 




Mannitol Hexanitrate NS 






melting point 
112 °C 


boiling point 
explodes at 160 °C 


mannitol hexanitrate 


molecular mass 
452.17 g/mol 


density 

1.230-1.604 g/ 
mL 


table key 


sensitivity 

low 


chemical formula 
C 6 H 8 N 6°18 


explosive velocity 
7000 m/s 


estimated cost 

$?.00/g 





ch 2 ono 2 

o 2 no-c-h 

o 2 no-c-h 

h-c-ono 2 

h-c-ono 2 

ch 2 ono 2 





Mannitol hexanitrate, or nitro mannitol, is a somewhat unstable primary explosive compound. Nitro 
mannitol is prepared by nitrating the sugar mannitol. Mannitol or, mannite, is not your everyday sugar so 
do not expect to find any in the grocery store. Mannitol comes in two stereoisomeric forms called L- 
mannitol and D-mannitol. A stereoisomer is a pair of molecules that are mirror images of each other, 
same formula but arranged differently. Like your hands they are equal but opposite. When a beam of 
polarized light passes through a solution of a stereoisomer and the angle changes, it is optically active. 
Polarized light are beams of light traveling in the same plane, sunglasses polarize light so only light 
waves of one plane, usually vertically, reach your eyes. If vertical light is rotated to horizontal the angle 
has changed. Light rotated left is called levorotatory, abbreviated L. Light rotated to the right is called 
dextrorotatory, abbreviated D. Why the lecture? First of all I love stereoisomerism, and second there is 
always a chance that chemicals will react differently if L and D. Now you know. In all probability the L 
or D mannitol will synthesize nitro mannitol. The difference commonly affects biological reactions. This 
explosive was first prepared back in 1847 by A. Sobrero when he mixed mannitol with nitric acid. It was 
prepared on a lab scale throughout the 19th century and was manufactured in the Royal Arsenal at Turin, 
Italy until 1853 when it blew up. Mannitol hexanitrate is also called nitromannite or hexanitromannite, 
the French call it nitromannitane, the Germans and Italians call it nitromannite, and the Russians call it 



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Megalomania's Method of Making Mannitol Hexanitrate 



mannitazotnokislyy. Mannitol hexanitrate is used as a secondary explosive and in some cases as a safety 
blasting cap. It can be stored safely with the addition of 5-10% sodium, potassium, or lithium salicylates. 



CHEMICALS 


APPARATUS 


ethyl alcohol 


dropping funnel/buret 


mannitol 


300-mL Erlenmeyer flask 




nitric acid 


graduated cylinder 


sodium bicarbonate 


sintered-glass funnel 


sulfuric acid 


thermometer 


water 



Cool 50 mL of 99% nitric acid in a 300-mL Erlenmeyer flask to 0 °C in a salt-ice bath. Slowly add 10 
g of mannitol in small amounts at such a rate as to keep the temperature below 0 °C. After all the 
mannitol is dissolved, add 55 mL of 99% sulfuric acid from a dropping funnel , or buret , at such a rate 
that the temperature is held below 0 °C. The porridge-like mass is filtered on a sintered- glass funnel , 
washed with water , 5% sodium bicarbonate , and again with water. The crude product is dissolved in 
warm sthyl alcohol , filtered, and cooled to deposit crystals of pure mannitol hexanitrate. A second crop 
is obtained by heating the filtrate and washings to boiling, adding water until the solution is cloudy, and 
cooling. The yield is 23 g or 96.6% of the theoretical yield. You will need a raduated cylinder for 
measuring liquids, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making MEDINA 






melting point 
104 °C 


boiling point 
explodes at 300 °C 


MEDINA 


molecular mass 
136.17 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
CH 4 N 4 O 4 


explosive velocity 
8700 m/s 


estimated cost 

$?. 00 /g 







NHN0 2 

ch 2 

nhno 2 









MEDINA stands for methylene dinitramine, and is also called methylenedinitramine and N,N- 
dinitromethanediamine. This compound was first prepared around 1949 at the University of Bristol by 
the hydrolysis of hexamine. This compound is not cruelty free (heh heh), it has been sprayed into rabbit 
eyes and injected under guinea pigs skins. The compound has been found to be non-toxic. This lab does 
not exactly fit in well with normal laboratory procedures as this information is the industrial laboratory 
method. Since this is the industrial method and it is still made in the lab I conclude this substance is 
either not used much or is to dangerous, I am leaning towards not used much. This is surprising as this 
explosive is quite powerful for such a small and simple molecule. Its real fault lies in the fact that it does 
not keep well, so use it soon after preparing. 





CHEMICALS 


APPARATUS 


acetic anhydride 


50 & 250-mL beaker 


acetone 


buret 


charcoal 


2-L Florence flask 


ethyl acetate 


graduated cylinder 


ethyl alcohol 


stirrer/stirring rod 




ethyl chloride 


thermometer 



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Megalomania's Method of Making MEDINA 



formamide 
formic acid 
isopropyl alcohol 
methenamine 
nitric acid 
2-nitropropane 
paraffin 

sodium hydroxide 
sodium sulfate 
water 
xylene 



This is a three step process for the manufacture of MEDINA: In a round bottom Florence flasl , 
mix 476 mL of firm amide and 70 g of methenamine . The flask is set up for refluxing, and heated at 140 
°C for 5 hours. It is then chilled in ice, the solid is filtered, and washed on a filter with 90 g of 
formamide. The crude product of methylenediformamide may be used in the next step or purified by 
dissolving in ethyl alcoho , decolorizing with charcoal , and chilling. 

19 mL of 100% nitric acid is added drop wise with a buret while stirring to a suspension of 5 g of 
crude methylenediformamide in 19 mL of acetic anhydride cooled to 10-15 °C in a iO-mL beaker . The 
solution is then held at 0 °C for 2 hours, and poured with stirring into a 50-mL beaker filled with 150 
mL of ice water . The precipitate is filtered, washed twice by mixing with ice water, pressed dry on the 
filter, and dissolved in 30 mL of ethyl acetate . The solution is seperated from water, dried over 
anhydrous sodium sulfate , concentrated in vacuum, 10 mL of isopropyl alcohol is added, and the 
product is collected. The product is methylene di(nitroformamide), which can be purified by 
recrystallization from either acetone , isopropyl alcohol, or from boiling ethyl chloride . 

The crude methylene di(nitroformamide) is pressed dry on the filter, stirred into 105 mL of formic 
aci , and the paste is allowed to stand overnight. The next day the solution is filtered through an acid 
filter, the formic acid and water is removed by distilling with xylene , and the crude MEDINA, which 
seperates as a sand, is filtered and dried over paraf fin and sodium hydroxide in vacuum. The crude 
MEDINA is recrystallized from -nitropropane or a 9: 1 solution of ethyl chloride/isopropyl alcohol. 

You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, 



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Megalomania's Method of Making MEDINA 



and a hermometer to monitor the temperature. 




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Megalomania's Method of Making MEDNA 




MEDNA 






melting point 


boiling point 


MEDNA 


molecular mass 


density 


table key 


sensitivity 

high 


chemical formula 
CH 4 N 4 O 4 


explosive velocity 


estimated cost 







MEDNA is an acronym for methylenediisonitrosoamine, it is also called N,N' 
dinitrosomethanedihydroxylamine. The information here is actually for the explosive salts of MEDNA 
as the free acid is unstable, there are several of importance. The sodium salt would seem to be of greatest 
importance with other salts being derived from it. The other salts include barium, cadmium, calcium, 
cesium, copper, monohydroxylamine, iron, lead, mercury, potassium, rubidium, silver, thallium, and tin. 
Of these, I have information for the barium, calcium, lead, potassium, silver, and sodium salts. All of 
these explosives are rather sensitive to shock, friction, and heat. They are usually used as detonators in 
mixtures with other common explosives. The sodium salt was first discovered around 1894. 





CHEMICALS 


APPARATUS 


acetic acid 


various beakers 


acetone 


Buchner funnel 




barium chloride 


graduated cylinder 


calcium chloride 


stirring rod 





ethyl alcohol 



thermometer 



nitric oxide 



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Megalomania's Method of Making MEDNA 



potassium iodide 
silver nitrate 
sodium 
water 



Barium MEDNA 

The barium salt of MEDNA is precipitated by adding barium chloride to a solution of either sodium or 
potassium MEDNA. This compound has the least explosive power of all the salts. 

Calcium MEDNA 

The calcium salt of MEDNA is prepared by adding calcium chloride solution to a solution of sodium 
MEDNA, thus precipitating out the calcium MEDNA. I have no other information on its explosive 
properties. 

Lead MEDNA 

The lead salt of MEDNA can be precipitated by adding a lead salt solution, such as lead acetate, lead 
chlorate, lead perchlorate, or lead nitrate, to a solution of sodium MEDNA. This explosive detonates at 
250 °C. It can be mixed with lead picrate or lead styphnate for use in detonators. 

Potassium MEDNA 

Prepare a solution of 56. 1 g of silver nitrate in 150 mL of wate: in a small beaker . Add this solution to a 
solution of 30 g of sodium MEDNA in 150 mL of water. The curdy silver salt is collected on a Buchner 
funnel, and washed on the filter paper with 450 mL of water. The damp salt is suspended in 200 mL of 
water, and the suspension is added slowly with stirring to a solution of 33.2 g of : o ssium iodide in 150 
mL of water. The mixture is stirred for 3 hours, and allowed to stand for 16 hours more. A precipitate of 
silver iodide is filtered off, and the water is removed from the remaining solution in vacuum to give 
about 18.8 g of impure potassium MEDNA. This solid is dissolved in 50 mL of hot water, clarified with 
Celite, and cooled to 0 °C. A small amount of solid is filtered off, and the water is evaporated in vacuum 
to give 13.5 g of an almost white solid, this corresponds to approximatly 61% of the theoritical yield. 

Silver MEDNA 

The silver salt of MEDNA is made as above by simply adding silver nitrate solution to the sodium salt 
of MEDNA without the potassium iodide. 

Sodium MEDNA 

Very slowly add 13.8 g of sodium metal in small portions to 300 mL of anhydrous ethyl alcohol and 
cool to 6 °C under nitrogen (If you have some sodium ethoxide handy that would do the trick since that 
is what this reaction makes, it is also safer). 38.4 g of acetone is added slowly with vigerous stirring as 



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Megalomania's Method of Making MEDNA 



nitric oxide is passed in at 320 mL per minute for 140 minutes. A fine yellow solid should form and is 
collected on a Buchner funnel, then the damp solid is dissolved in 130 mL of water, made slightly acidic 
with glacial acetic acid , and heated on a steam bath until gassing ceases to come from the solution. The 
mixture is poured into 400 mL of ice cold ethyl alcohol to give 25.3 g of a brown solid which is 
recrystallized twice from a 2:1 ratio of ethyl alcohol and water to give a white solid which decomposes 
without melting at 225-260 °C. 




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Megalomania's Method of Making MeEDNA 






melting point 


boiling point 


MeEDNA 


molecular mass 


density 




120.5 °C 


explodes at 360 °C 


164.13 g/mol 


? g/mL 




table key 


sensitivity 


chemical formula 


explosive velocity 


estimated cost 




high 


C 3 H 8 N 4 U 4 


? m/s 


$?. 00 /g 


A 










MeEDNA is an acronym for N-methylethylenedinitramine or N-methylEDNA. It was first prepared 
back in 1888, but did not gain interest until World War II. This explosive seems to have good stability, 
resists decomposition, and does not vaporize much. MeEDNA has about 120% the explosive power of 
TNT. 



A 



CHEMICALS 


APPARATUS 




acetic anhydride 


dropping funnel 




ammonium hydroxide 


500-mL Florence flask 


benzene 


stirrer 


ethylene dichloride 


thermometer 






hydrochloric acid 


3-nitrazabutylamine 


nitric acid 



Prepare a solution of 82.4 g of 3-nitrazabutylamine in 100 mL of dry benzene in a 3-necked 500-mL 

Florence flask fitted with a stirrer , a dropping funnel , and a thermometer . Cool the solution in a salt-ice 



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Megalomania's Method of Making MeEDNA 



bath, and add 75 mL of acetic anhydride drop wise. A white solid precipitate should form and is collected 
and dried to give 71 g of N-acetyl-N'-methyl-N'-nitroethylenediamine, melting point 79-80 °C. 20 g of 
this compound is added in small portions to a mixture of 100 mL of 100% nitric acid and 100 mL of 
acetic anhydride cooled to -10 to -5 °C. The mixture is stirred for 45 minutes, poured onto crushed ice, 
the solid is filtered, washed with water, and finally dried to give a yield of 9.5 g of N-acetyl-N’-methyl- 
EDNA, melting point 55-56 °C. To 7.6 g of this compound, add 25 mL of 14% ammonium hydroxide , 
whereupon it dissolves with evolution of heat. The solution is cooled, acidified with dilute ydrochloric 
acid , the precipitated solid is collected on a filter, washed with water, and dried to give 5.1 g of 
MeEDNA which corresponds to a yield of 84.3%. The MeEDNA can be purified by recrystallizing from 
ethylene dichloride . 




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Megalomania's Method of Making Mercurous Nitratophosphite 




Mercurous Nitratophosphite 




melting point 
explodes at 100 °C 


boiling point 


mercurous nitratophosphite 


molecular mass 
546.24 g/mol 


density 
? g/mL 


table key 


sensitivity 

medium 


chemical formula 
HgN0 3 Hg(H 2 P0 2 )H 2 0 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





t 

NH 


:■ H a O 

h Hg+ J 

T 


ii 

>■- Hg+ 
^0- 
H 









Mercurous nitratophosphite was first prepared by S. Hada in 1895 by the lab presented here. This 
explosive will decompose in water, or when wet, with the release of mercury vapor, so I suggest keeping 
it tightly stoppered and away from moisture, or even better in a desiccator to get the moisture. 

Mercurous nitratophosphite will explode when heated to 100 °C, or when it comes in contact with a hot 
wire. I do not know if shock and friction affect it. Further information about this compound is 
unavailable. 



CHEMICALS 


APPARATUS 




mercuric oxide 


beaker 




mercury 


Buchner funnel 




nitric acid 


desiccator 






potassium hypophosphite 



Prepare a solution of mercurous nitrate by dissolving mercuric oxide to saturation in nitric acii , and 
then shake violently with metallic mercun for a few minutes. Mercurous nitratophosphite can be 
prepared by adding a fairly concentrated solution of )otassium hypophosphite to a solution of mercurous 
nitrate in a small beaker , avoiding an excess of the hypophosphite. As the mercurous nitratophosphite 
precipitate decomposes when left in contact with the mother liquor, it must be filtered and dried 



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Megalomania's Method of Making Mercurous Nitratophosphite 



immediately by vacuum filtration on a 3uchner funnel without washing to drive away any moisture. It 
can be dried and stored in a vacuum desiccator. 




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2004 



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Megalomania's Method of Making Mercury Fulminate 




Mercury Fulminate^ 






melting point 
explodes at 150 °C 


boiling point 


mercury fulminate 


molecular mass 
284.62 g/mol 


density 
2.5 g/mL 


table key 


sensitivity 
very high 


chemical formula 
Hg(ONC) 2 


explosive velocity 
4000 m/s 


estimated cost 

$?.00/g 







O' O' 

"C=N + Hg2+ + N=C' 


C®> 



Mercury fulminate is an unstable primary explosive compound. It was first prepared in the late 
seventeenth century by Johann Kunckel von Lowenstern by a procedure very similar to the modern 
method presented here. Lowenstern detailed mercury fulminate synthesis in his posthumously written 
Laboratorium Chymicum, he used aqua fortis, spiritum vini, and in fimum equinum. That last one is 
horse manure if you wanted to know. Mercury fulminate was first patented by Alfred Nobel in 1867 for 
blasting caps. It is not used today for that purpose because of more stable explosives from modern 
chemistry. Its manufacture is not complicated nor the chemicals in its makeup rare. Mercury can be 
extracted from a variety of products but it is very expensive. Only a chemical supply company could 
provide mercury in useful quantities. This lab produces nitrogen dioxide gas as a byproduct, this is a 
heavy red colored gas that is extremely toxic. The gas will turn moisture in your lungs to nitric acid and 
may cause fabric to ignite! This lab should be done outside or in a fume hood if possible. 





CHEMICALS 


APPARATUS 




acetic acid 


500-mL beaker 




ammonium hvdroxide 


desiccator 


ethyl alcohol 


lOOmL Erlenmeyer flask 


mercury 


graduated cylinder 






nitric acid 



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Megalomania's Method of Making Mercury Fulminate 




In a lOOmL Erlenmeyer flask , measure out 35 mL of 70% nitric acid , then add 5 g of mercury metal. 
This mixture should be left alone without shaking or stirring until all the mercury dissolves. Toxic gas 
will be produced. Keep the flask in a well ventilated area, or stopper the flask and lead a length of rubber 
tubing into water to safely dissolve the fumes. In a 500-mL beaker , place 50 mL of 90% ethyl alcohol , 
then add the acid-mercury mix in a well ventilated area. The temperature of the mixture will rise, a 
vigorous reaction will commence, white fumes will be released, and crystals of mercury fulminate 
should begin to precipitate. Red fumes of nitrogen dioxide will appear as the precipitation becomes more 
rapid, then white fumes again as the reaction moderates. After about 20 minutes the reaction should be 
over. Add water to the beaker and carefully decant off most of the water without losing any crystals. 

Add water and decant several times until the wash water is no longer acid to litmus. Finally, pour the 
neutral solution over a filter to collect the grayish-yellow crystals of mercury fulminate. The product 
may be purified by dissolving in strong ammonium hydroxide , filtering, and re-precipitating by the 
addition of 30% acetic acid . The pure fulminate is filtered off, washed with cold water, and stored in a 
container filled with water. Dry in a desiccator immediately before use. You will need a graduated 
cylinder for measuring liquids. 




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Megalomania's Method of Making 2-Methyl-2-Nitro- 1 -Propanolnitrate 




2-Methyl-2-Nitro-1 -Propanolnitrate 




melting point 
decomposes at 200 °C 


boiling point 


2-methyl-2-nitro-l -propanolnitrate 


molecular mass 
164.14 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
CH 3 C(N0 2 )2CH 2 0N0 2 


explosive velocity 
? m/s 


estimated cost 
$?.00/g 





no 2 ono 2 



This explosive comes from a study of nitroparaffin explosive derivatives done in 1941. This material is very 
resistant to heat, shock, friction, etc., it even resists blasting caps thus requiring a larger charge to detonate. 
Unfortunately it has poor stability after it is synthesized, it will not explode, but it will decompose. It has been 
deemed unworthy in the eyes of the military because of this. Otherwise it has 75% the power of nitroglycerine, 
it causes headaches like nitroglycerine, and it can gelatinize nitrocellulose pretty good. 





CHEMICALS 


APPARATUS 




ethyl ether 


500-mL Erlenmever flask 


2-methyl-2-nitro- 1 -propanol 


graduated cylinder 




nitric acid 


separatory funnel 


sodium bicarbonate 


stirrer/stirring rod 


sulfuric acid 


thermometer 




water 


vacuum desiccator 





Prepare a mixture of 40 mL of 90.5% nitric acid and 130 mL of 103% sulfuric acid (oleum with 3% sulfur 
trioxide) in a 500-mL Erlenmeyer flask , and cool to 15 °C in a salt-ice bath. Slowly add, with fast stirring, 50 g 
of 2-methyl-2-nitro- 1-propano to the acid mix while maintaining the temperature as close to 15 °C as possible. 
Continue stirring for 1 hour after the addition then let it stand for 15 minutes. Pour the contents of the flask over 
some crushed ice to separate the product. Add this mixture to a se aratory funne where the bottom layer of 
spent acids can be removed. Wash the remaining product with water , sodium bicarbonate solution, and again 



(§> 



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Megalomania's Method of Making 2-Methyl-2-Nitro- 1 -Propanolnitrate 



with water until the washings are neutral to litmus. Combine the washings with the spent acid and extract with 
ethyl ether to obtain additional product. Wash the ethyl ether until neutral to litmus and add it to the main 
product. Allow the ethyl ether to evaporate and dry the residue in a vacuum desiccator . The yield is about 50%. 
You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a 
thermometer to monitor the temperature. 



■COMMrNTlB 



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Megalomania's Controversial Chem Lab ©1997-2004 /2-methyl-2-nitro-l -propanolnitrate/ revised January 31, 
2004 



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Megalomania's Method of Making Metriol Trinitrate 




melting point 
-3 °C 


boiling point 
decomposes at 182 °C 


metriol trinitrate 


molecular mass 
255.15 g/mol 


density 
1.47 g/mL 




table key 


sensitivity 

high 


chemical formula 
CH 3 C(CH 2 0N0 2 ) 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 





Metriol trinitrate, also called MTN; 1,1,1-trimethylolethane trinitrate; nitropentaglycerin; 1,3- 
propanediol, 2-methyl-2-[(nitrooxy)methyl]-, dinitrate (ester); 2-Methyl-2-hydroxymethyl- 1,3- 
propanediol trinitrate; and metriolo in Italian, was first prepared and patented by the Bombrini-Parodi- 
Delfino Co of Italy under the name Metriolo. The Germans got wind of Metriolo before WWII and saw 
that it was a good flash and erosion reducing agent, so they began to manufacture it. Metriol trinitrate is 
a powerful liquid explosive that is somewhat sensitive to explosion, about as much as nitroglycerin. It 
has been used as a flash and corrosion reducing additive in propellants and as an ingredient in 
commercial explosives. 





CHEMICALS 


APPARATUS 




calcium chloride 


Erlenmever flask 




ethvl ether 


graduated cylinder 




metriol 


stirrer/stirring rod 




nitric acid 


thermometer 



http://www.roguesci.org/megalomania/explo/metriol_trinitrate.html (1 of 2)12-8-2004 17:26:13 





Megalomania's Method of Making Metriol Trinitrate 



sodium bicarbonate 
sulfuric acid 
water 



Prepare a mixture of 50 mL of concentrated (>90%) nitric acid and 20 mL of concentrated (>90%) 
sulfuric acid in a small Erlenmeyer flask, and cool to 20 °C in a salt-ice bath. Carefully add 3.5 g of 
metrit to the flask while maintaining a temperature of 20 °C. The mixture is stirred for 30 minutes after 
the addition, then cooled to 5 °C, and finally poured over ice. The solution is extracted with ethyl ether , 
the extract is washed with yater, and the wash is adjusted to pH 7 by shaking with sodium bicarbonate 
solution, then washed with water three more times. It is then dried with calcium chloride , poured over a 
filter to remove impurities, and freed of ethyl ether by bubbling with dry air until a constant weight is 
obtained. Yield is about 88%. You will need a graduated cylinder for measuring liquids, a stirring roc or 
magnetic stirrer for mixing, and a thermometer to monitor the temperature. 




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Megalomania's Method of Making MMAN 






melting point 

? °C 


boiling point 
230 °C 


MMAN 


molecular mass 
94.070 g/mol 


density 
1.2 g/mL 


table kev 


sensitivity 

low 


chemical formula 

ch 3 nh 3 ono 2 


explosive velocity 
6100 m/s 


estimated cost 

$?.00/g 





O' 

NH 3 + lit 

'O'" 

■H 



MMAN is an acronym for monomethylamine nitrate, it is also called methylamine nitrate. It is a 
powerful and stable primary explosive compound. Its stability makes it a better choice for a primary 
explosive and as a test of the independent chemist's skill. When used as a blasting cap it will probably 
require some other more sensitive material to help it along, but when it explodes it will detonate even 
insensitive explosives. The only problem with it is that it is a hygroscopic compound, so keep it very 
tightly sealed in storage. Another snag is the methylamine solution used, it is not a supermarket item 
now that drug dealers have made it a DEA watched chemical, it is easy to make though. A note on nitric 
acid: You can use any concentration of acid from 20% and up, it is the volume of acid that is required. I 
have given the volume for pure acid, adjust as needed for lesser solutions. 





CHEMICALS 


APPARATUS 


methvlamine 


1000-mL beaker 


nitric acid 


desiccator 


graduated cylinder 


stirrer/stirring rod 





http://www.roguesci.org/megalomania/explo/MMAN.html (1 of 2)12-8-2004 17:26:14 




Megalomania's Method of Making MMAN 



Place 250 mL of 33% methylamine solution in a 1000-mL beaker . Slowly add, with stirring, 385 mL 
of 100% nitric acid . It will be helpful to divide the acid into four equal portions of 96 mL each and use a 
salt-ice bath. The acid addition will generate substantial heat and may boil, wait until the solution cools a 
little before adding the next portion. It is not necessary to add concentrated nitric acid, a concentration as 
low as 20% will suffice. You must still add the equivalent of 385 mL of pure acid. Remember there is 1 
mL of pure acid per 1% of solution in 100 mL. A 20% solution would require 1925 mL. After adding 
the acid, test the solution with pH paper, or litmus paper. The result must be near pH 7 if using the pH 
paper and be neutral if using litmus paper. If the solution is acidic add methylamine until pH 7 is 
reached. If the solution is basic add nitric acid until pH 7 is reached. Evaporate the liquid to precipitate 
the crystals of MMAN by heating until a slurry is reached, then use vacuum drying to remove the rest of 
the water. Because the MMAN is hygroscopic, it will be impossible to drive off all the water unless 
heated under vacuum or placed in a desiccator . Extreme care must be taken when heating an explosive 
IT CAN EXPLODE. MMAN is safe enough that it only burns when strongly heated. Use either a 
hotplate, steam bath, or oil bath to heat the explosive. If you have access to vacuum equipment use the 
vacuum drying method. Y ou will need a graduated cylinder for measuring liquids, and a stirring rod or 
magnetic stirrer for mixing. 




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Megalomania's Method of Making NIBGkDN 






melting point 
37.4 °C 


boiling point 
decomposes at 200 °C 


NIBGkDN 


molecular mass 
225.12 g/mol 


density 
? g/mL 


table key 


sensitivity 

high 


chemical formula 
CH 3 C(N0 2 )(CH 2 0N02)2 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 






NIBGkDN is an acronym for nitro-iso-butylglycol dinitrate. This substance is more commonly called 
nitromethylpropanediol dinitrate, and a more scientific name is 2-methyl-2-nitro- 1,3 -propanediol 
dinitrate. It was made on a lab scale by Germany in WWII and has not really found its way into the 
industrial mainstream as it has been designated too unstable for military use. It was proposed for use in 
commercial explosives as a substitute for nitroglycerine. It is a white waxy solid that is very sensitive to 
impact and has low tolerance for heat. Its explosive power is comparable to other detonating 
compounds. 









CHEMICALS 


APPARATUS 




ethyl ether 


beaker 




2-methyl-2-nitro- 1,3-propanediol 


300-mL Erlenmeyer flask 




nitric acid 


graduated cylinder 




sodium sulfite 


seperatory funnel 








sulfuric acid 


stirrer/stirring rod 




water 


thermometer 



http://www.roguesci.org/megalomania/explo/NIBGkDN.html (1 of 2)12-8-2004 17:26:15 





Megalomania's Method of Making NIBGkDN 



vacuum desiccator 



Gradually sift 50 g of dry, ground -methyl-2-nitro-l, 3-propanediol into a mixture of 80 mL of 100% 
nitric acid and 98 mL of 100% sulfuric acid with mechanical stirring at a temperature of about 15 °C in a 
300-mL Erlenmeyer flask . After the addition, the temperature is allowed to rise to 20 °C and is kept 
there for 30 minutes with stirring. Let the mixture stand for 1 hour, then transfer it to a separatory funnel 
where the heavier spent acid layer can be drawn off. The remaining oil is washed twice with aqueous 
sodium sulfite solution heated to around 45 °C, and then with warm water until neutral to litmus paper. 
Transfer the liquid to a beake: and dry under vacuum at 50 °C, the oil is chilled until it becomes milky in 
appearance and waxy crystals separate. An additional amount of material can be obtained by mixing all 
the washings and spent acid then extracting with ethyl ether . The ethyl ether is separated and washed 
with water. The ethyl ether is allowed to evaporate and the residue is dried in a vacuum desiccator . Their 
should be an additional 16.2% of product. Total yield is 92.2% altogether. You will need a graduated 
cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to 
monitor the temperature. 




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Megalomania's Method of Making NIBGTN 




NIBGTN s 




melting point 
-50 °C 


boiling point 
decomposes at 180 ° C 


NIBGTN 


molecular mass 
286.12 g/mol 


density 
1.64 g/mL 


table key 


sensitivity 

high 


chemical formula 
0 2 NC(CH 2 0N0 2 ) 3 


explosive velocity 
7860 m/s 


estimated cost 

$?.00/g 





NIBGTN is an acronym for nitroisobutylglycerol trinitrate. The proper name for this compound is 
1,3 -propanediol, 2-nitro-2-[(nitrooxy)methyl]-, dinitrate (ester). Other names include 1,3-propanediol, 2- 
(hydroxymethyl)-2-nitro-, trinitrate (ester); nitroisobutanetriol trinitrate; 1,3-propanediol, 2-nitro-2- 
[(nitrooxy)methyl]-, dinitrate; 1,3 -propanediol, 2-(hydroxymethyl)-2-nitro-, trinitrate; nitroisobutyl 
glyceryl trinitrate; nitroisobutyl glycol trinitrate; nitroisobutylglycerintrinitrate; and trimethylol 
nitromethane trinitrate. This compound is a viscous, yellow, oderless, oily liquid similar to 
nitroglycerine. This compound was first experimented on back in 1912, and the current method of 
preperation was developed by Dr. A. Stettbacher in 1934. It was proposed to use NIBGTN as a 
substitute for nitroglycerin in commercial explosives, but its greater instability and poor thermal stability 
made it difficult to work with. The detonation velocity listed above can be achieved only by confining 
the explosive and using a powerful detonator, otherwise the detonation velocity is a rather low 1000- 
1500 m/s. 



CHEMICALS 



APPARATUS 



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Megalomania's Method of Making NIBGTN 



ethyl ether 


500-mL Erlenmeyer flask 




nitric acid 


graduated cylinder 


tris(hydroxymethyl)nitromethane 


separatory funnel 


sodium bicarbonate 


stirrer/stirring rod 


sodium sulfite 


thermometer 


sulfuric acid 


vacuum desiccator 


water 



Prepare an acid mixture of 99.1 mL of 99% sulfuric acid and 76.3 mL of 99% nitric acid in a iOO-mL 
Erlenmeyer flask , cool this mixture in a salt-ice bath. Slowly add, with stirring, 50 g of tris 
(hydroxymethyl)nitromethane to the flask while keeping the temperature below 15 °C. The addition 
should take about 30 minutes. Stir the mixture for an additional 30 minutes while allowing the 
temperature to drop to 5 °C. Transfer the contents of the flask to a separatory funne and allow it to stand 
for several minutes while the layers separate, then draw off the bottom layer of acid. Wash the remaining 
oil with watei , then with lodiuin bicarbonate solution, and finally twice more with water. The washed oil 
should be neutral to litmus, if not, wash with more water until it is. Combine all of the washings and mix 
them with the spent acid. Cool this mixture and extract it several times with ethyl ether to remove 
additional product. Wash the ethyl ether extracts with water, evaporate the ethyl ether, and add the 
remaining product to the other washed product. Dry all of the NIBGTN in a vacuum desiccato . The 
yield is around 95%. Sometimes the NIBGTN will form an emulsion that can take awhile for layers to 
separate fully, this can be mitigated by heating all wash water to 43.5 °C, using concentrated sodium 
sulfite solution instead of sodium bicarbonate, and bubbling in compressed air while washing. You will 
need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a 
thermometer to monitor the temperature. 




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Megalomania's Method of Making NIBGTN 



Megalomania's Controversial Chem Lab ©1997-2004 /NIBGTN/ revised January 31, 2004 




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Megalomania's Method of Making Nitrated Petroleum 





This explosive procedure intrigues me because what chemical can be more readably available than 
gasoline, or for that matter motor oil, kerosine, and diesel. The nitration of petroleum generally produces 
either brown non-crystalline solids or liquid products that are explosive. The first attempts to nitrate 
petroleum were made in Russia at the end of the 19th century by one Dr. Konovaloff. Dilute nitric acid 
under pressure was used to nitrate the product, obtaining very low yields. In 1902 a nitration method 
patented by Edeleanu and Filti used mixed nitric-sulfuric acids, unfortunately for them no practical 
application of their patent was found. Others tried using different kinds of petroleum like A.S. Flexer, 
Freund, and Kharichkov to name a few. Not that it matters who they are, but I like to know. You may 
experiment yourself on everything from crude oil to that stuff you get at the hardware store for oil 
lamps. Things are screwed up nowadays, all of the good chemical additives that make petroleum 
nitrateable seem to be getting legislated by the government (only the democrat oppressors). This lab may 
have worked for scientists a hundred years ago, but it may not work for you today. 



A 



CHEMICAFS 


APPARATUS 


gasoline 


beaker 




nitric acid 


graduated cylinder 




sulfuric acid 


thermometer 






water 



http://www.roguesci.org/megalomania/explo/nitrated_petroleum.html (1 of 2)12-8-2004 17:26:17 




Megalomania's Method of Making Nitrated Petroleum 



Standard gasoline , get the cheap stuff and not gasahol (gas/ethyl alcohol mix) if you can avoid it, is 
added gradually to a mixture of 15 parts 100% sulfuric acid and 3 parts 100% nitric acid in a large 
beaker . Add 1 part of gasoline per 18 parts of mixed acid. The reaction temperature should be somewhat 
cool, never let the temperature rise above 80 °C. A temperature below 20 °C should do, you can regulate 
this with a salt-ice bath. When the nitration is completed, the mixture is diluted with a large quantity of 
cold water to precipitate the product. The un-nitrated oil will float to the top of the acid- water solution. 
Collect the precipitate on a filter and wash with water, yield will be 30% to 90% depending on the crude 
oil used to manufacture the gasoline. You will need a graduated cylinder for measuring liquids, and a 
thermometer to monitor the temperature. 




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Megalomania's Method of Making m-Nitrobenzenediazonium Perchlorate 




/77-Nitrobenzenediazonium Perchlorate 




melting point 
explodes at 154 °C 


boiling point 


m-nitrobenzenediazonium perchlorate 


molecular mass 
235.57 g/mol 


density 
? g/mL 


table key 


sensitivity 
very high 


chemical formula 
0 2 NC 6 H 4 NN(C10 4 ) 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 




(«} 



m-nitrobenzenediazonium perchlorate, also called m-nitrodiazobenzeneperchlorate, was first patented back 
in 1911 by the German scientist E. von Hertz for use in detonators. This compound is sensitive to shock and 
friction and will explode if heated to 154 °C. Although this compound is not very soluble in water, it will draw 
moisture out of the air being hygroscopic. This compound has been used as a detonator when mixed with 
nitromannite or other explosive nitric esters. 



CHEMICALS 


APPARATUS 


ethyl alcohol 


beaker 


ethyl ether 


graduated cylinder 


hydrochloric acid 


stirring rod 


m-nitroaniline 


test tube 


perchloric acid 




sodium nitrite 




water 





Suspend 0.5 g of m-nitroaniline in 5 mL of water in a wide test tube , then add 0.5 mL of concentrated 
hydrochloric acid and 2.2 mL of 20% rerchloric acid solution. After the nitroaniline has dissolved, 15 mL of 



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Megalomania's Method of Making m-Nitrobenzenediazonium Perchlorate 



water is added and the solution is cooled by immersing the test tube in a beaker filled with ice water. Prepare a 
solution of 0.25 g of odium nitrite dissolved in 1 or 2 mL of water, add this solution to the test tube in three or 
four portions, the mixture being shaken after each addition or stirred with a stirring rod the end of which is 
covered with a rubber policeman or piece of rubber tubing. After standing in the cold for 5 minutes, the material 
is filtered to collect it, and the feltlike mass of pale yellow needles is washed with cold water, then with ethyl 
alcohol , then with ethyl ether . The product should be allowed to dry in several small portions on different pieces 
of filter paper. You will need a graduated cylinder for measuring liquids. 




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Megalomania's Controversial Chem Lab ©1997-2004 /ra-nitrobenzenediazonium perchlorate/ revised January 
31, 2004 



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Megalomania's Method of Making 2-Nitro-2-(3',5'-Dinitrophenyl)-Propanediol-l,3 Dinitrate 




2-Nitro-2-(3',5'-Dinitrophenyl)-Propanediol- 



1,3 Dinitrate 




A 



A 



melting point 
115.2-115.8 °C 


boiling point 

? ° C 


2-nitro-2-(3',5'-dinitrophenyl)- 
propanediol- 1 , 3 dinitrate 


molecular mass 
377.19 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
(N0 2 ) 2 C 6 H 3 (N0 2 )(CH 2 0N0 2 ) 2 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 






This compound looks like flat rectangular crystalline plates or sometimes in the form of prisms. The 
explosive properties of this compound were discovered by R. McGill at the NDRC Research Lab in 
Bruceton, Pennsylvania. It is somewhat powerful, having 126% the strength of TNT, and has a 
somewhat low sensitivity to impact. 





CHEMICALS 


APPARATUS 




acetone 


beaker 


ethyl alcohol 


graduated cylinder 




nitric acid 


thermometer 






2-nitro-2-(3',5'-dinitrophenyl)-propanediol-l,3 


water 



http://www.roguesci.org/megalomania/explo/nitro_propanediol.html (1 of 2)12-8-2004 17:26:19 





Megalomania's Method of Making 2-Nitro-2-(3',5'-Dinitrophenyl)-Propanediol-l,3 Dinitrate 



Add 20 g of 2-nitro-2- ( 3 ’ ,5 dinitropheny l)-propanediol- 1 , 3 in several portions to 130 mL of fuming 
nitric ack in a small beaker , cooled to 5 °C with a salt-ice bath. After about 6 minutes all of the material 
should be dissolved and the temperature will have risen to 10 °C. Drown the mixture in 1.5 L of ice 
water and allow it to stand for 15 minutes. Decant off most of the ice water and collect the hardened, 
gummy material on a filter then wash it with water. Purify by dissolving in acetone and crystallize it by 
adding ethyl alcohol to the solution. The yield varies between 67% and 86%. You will need a graduated 
cylinder for measuring liquids, and a lermometer to monitor the temperature. 




Lab 


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Megalomania's Controversial Chem Lab ©1997-2004 /2-nitro-2-(3’,5'-dinitrophenyl)-propanediol-l,3 
dinitrate/ revised January 31, 2004 



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Megalomania's Method of Making Nitrogen Sulfide 




Nitrogen Sulfided 






X 

W"7 ? n 

z 1 

unknown 





Nitrogen sulfide, also called sulfur nitride, nitrogen tetrasulfide, tetranitrogen tetrasulfide, or 
Schwefelstickstoff, is a very unstable primary explosive compound. Its manufacture is hazardous and 
rather complicated, yet is has found some industrial uses in detonators, diesel fuel as an ignition 
promoter, pesticides, fungicides, and as an accelerator in rubber vulcanization. Nitrogen sulfide is 
sensitive to heat, friction, shock, and will explode if heated over 160°C if impurities are present. The 
chemicals used in this lab are not easily obtainable, but can be made by the home chemist. The main 
ingredient is sulfur dichloride, an unstable and toxic compound, benzene is also used but it is about as 
popular as a rapist at a feminist gathering. Its stigma is "carcinogen," not even labs use it much anymore, 
so now labs do not sell it, and no public store will carry such toxins. It is possible to use toluene or 

carbon tetrachloride instead. 



A 



CHEMICALS 


APPARATUS 


ammonia 


desiccator 


benzene 


Erlenmever flask 


sulfur dichloride 


graduated cylinder 



Dissolve 131 mL of freshly prepared sulfur dichloride in 1950 mL of benzene in a large Erlenmeyer 
flask . You may pour the solution through a filter to remove any impurities that may have been in the 
sulfur dichloride, but it is best to purify it beforehand. Bubble anhydrous ammonia gas through the 
solution. A brown precipitate will begin to form, continue adding ammonia until this precipitate 
dissolves and forms an orange-yellow solution. Now large amounts of ammonium chloride will 
precipitate out of solution. Carefully heat the benzene until it boils. Immediately pour this solution over 
a filter to remove the crystals, collect the filtrate. Wash the crystals with 200 mL of benzene and add the 



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Megalomania's Method of Making Nitrogen Sulfide 



wash to the filtrate. Allow the benzene filtrate to evaporate until a crystalline slush remains, filter the 
slush, and allow to dry. Using vacuum drying or a desiccator can speed the process. The resulting 
product should be yellow to orange-red crystals of nitrogen sulfide. You will need a graduated cylinder 

for measuring liquids. 




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melting point 
178 °C 


boiling point 
decomposes at 185 °C 


nitrogen sulfide 


molecular mass 
184.27 g/mol 


density 
2.22 g/mL 


table key 


sensitivity 

high 


chemical formula 
N 4 S 4 


explosive velocity 
? m/s 


estimated cost 

$?. 00 /g 



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Megalomania's Method of Making Nitrogen Trichloride 




A 




melting point 
-27 °C 


boiling point 
71 °C 


nitrogen trichloride 


molecular mass 
120.38 g/mol 


density 
1.653 g/mL 


table key 


sensitivity 
very high 


chemical formula 
NC1 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 







Cl 

Cl Cl 









Nitrogen trichloride, also called nitrogen chloride, agene, chlorine nitride, trichloramine, trichlorine 
nitride, chloride of azode, or Stickstofftrichlorid, is an unstable primary explosive compound. Its 
preparation is not complicated and the chemicals used are simple, cheap, and readily obtainable. You 
could pump the stuff out by the liter if it was not so sensitive. Nitrogen trichloride will explode if heated, 
exposed to sunlight, or mixed with organic compounds. It does not like to be friendly around many other 
chemicals, shock, sparks, and it will explode if frozen and thawed. The explosive properties were first 
reported in the 18th century by Sir H. Davy, he had this to say: "The fulminating oil which you 
mentioned roused my curiosity and nearly deprived me of an eye. After some months of confinement I 
am again well." Ouch, that must have hurt. 





CHEMICALS 


APPARATUS 




ammonium nitrate 


bubbler 


chlorine 


200-mL Erlenmever flask 


water 


graduated cylinder 


medicine dropper 



Dissolve 30 g of ammonium nitrate in 70 mL water in a 200-mL Erlenmeyer flask . Prepare a chlorine 

generator as described in the synthesis section. Place a tube connected to the generator at the bottom of 
the flask so the chlorine gas can bubble into the liquid, a bubbler will help a lot with the reaction. Gently 
heat the flask to start the reaction while adding chlorine gas. An oily yellow liquid will begin to appear 



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Megalomania's Method of Making Nitrogen Trichloride 



on the bottom of the flask, that is the nitrogen trichloride. Stop heating the flask when the drops appear. 
After 20 to 30 minutes the reaction should be complete. Use a medicine dropper to extract the nitrogen 
trichloride from the flask, transfer it to a small test tube and remove any water accidently sucked up with 
it. You will need a graduated cylinder for measuring liquids. This explosive will decompose within 24 
hours of its preparation. 




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Megalomania's Method of Making Nitrogen Triiodide 




melting point 


boiling point 


nitrogen triiodide 


molecular mass 
394.77 


density 
? g/mL 


table key 


sensitivity 
very high 


chemical formula 

ni 3 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 



I 




1 

I ^1 






Nitrogen triiodide, also called ammonium triiodide, is a very unstable explosive that's not really 
practical due to its tremendous instability and cost. When wet it is stable but when dry the touch of a 
feather can cause it to detonate. Wet nitrogen triiodide should be spread out as much as possible or 
numerous small piles made. When dry the nitrogen triiodide will not explode from its own weight if 
spread out, a single large pile will. 



A controlled lab demo using a feather to cause detonation: 



aJUjIH 



The high cost of iodine, anywhere from $60 to $100 for a 500 g bottle, and its rarity, make it impractical 
from an economic standpoint. Those useless anarchist texts say iodine can be purchased in drug stores, it 
is sold in very tiny amounts heavily diluted with alcohol. The drug dealers have made iodine a restricted 
chemical, very few drug stores even carry it now, there are safer alternatives. The simplicity in which 
this explosive can be made gives wanna be punks an excuse to try. THIS EXPLOSIVE IS ONLY A 
CURIOSITY AND SHOULD NEVER BE MADE EXCEPT FOR A CONTROLLED 
DEMONSTRATION AS ABOVE! Stories abound about the dangers and ease of making nitrogen 
triiodide. There was a senior undergraduate student (no not me) given full access to a lab who made 
some, it exploded in a beaker showering him with glass. He was not wearing safety goggles. By some 
miracle the glass embedded in his face did not rip his eyes to shreds. Then there were the teenage 



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Megalomania's Method of Making Nitrogen Triiodide 



hoodlums that stole some iodine from their high school chem lab, made the nitrogen triiodide at home, 
and brought it back to school. With a pop and puff of purple gas the teacher knew what it was. A word 
of advise to them for next time: Leaving the instructions on top of your desk in full view of teach will 
save you a lot of time scrubbing iodine stains during your next suspension. It is best to leave it dry where 
you want to detonate it ASAP. 



CHEMICALS 


APPARATUS 


ammonium hydroxide 


beaker 




iodine 


stirring rod 


water 


graduated cylinder 



Nitrogen triiodide is formed when iodine atoms displace the hydrogen atoms in ammonia NH 3 + I = 
NI 3 . This reaction occurs when iodine crystals, I 2 are soaked in excess ammonium hydroxide. To begin, 
select a small beakei or even a disposable cup about 50-mL in capacity. This process may permanently 
stain any container so I suggest the cup. Add 2 g of iodine crystals to the beaker, crush them as much as 
possible with a stirring rod . Add 40 mL ammonium hydroxide to the beaker. After 2 hours the reaction 
should be complete. Pour the solution over a filter to collect the crystals, any excess can be rinsed out of 
the beaker with water . Put the crystals where you want them immediately because there only semblance 
of stability is when wet. Drying will take about 1 hour. You will need a graduated cylinder for 
measuring liquids. 




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Megalomania's Method of Making Nitroglycerin 




melting point 


boiling point 


nitroglycerin 


molecular mass 


density 


13.5 °C 


decomposes at 50-60 °C 


227.09 g/mol 


1.5918 g/mL 


table key 


sensitivity 
very high 


chemical formula 
C 3 H 5 N 3°9 


explosive velocity 
7700 m/s 


estimated cost 

$?.00/g 



A 





ch 2 — ono 2 

CH— 0N0 2 

ch 2 -ono 2 





Nitroglycerin was first prepared by a scientist named A. Sobrero around 1847 where it was used as a 
medicine. It was then mass produced by the great scientist Alfred Nobel in 1864 when he developed 
improvements on its synthesis and a method of detonating it. The devastation nitroglycerin caused on 
both the battlefield and the factory earned Nobel the title "Merchant of Death." Nobel was haunted by 
the lives nitroglycerin claimed so he created the Nobel Peace Prize to honor champions of peace, and 
later, supreme accomplishments in science. His exposure to nitroglycerin gave him constant agonizing 
headaches, and ironically he took nitro pills for a heart condition later in life. Nitroglycerin remains in 
use as a medicine, but not for explosives. Nitroglycerin is a very unstable high explosive compound. The 
first time I tried to make nitroglycerin was back in my early undergraduate days. I was impatient and 
decided to make some in the dorm without observing proper safety procedures. I was out of ice. Let me 
just say how important it is to keep this lab cool and slow. Nitrogen dioxide, a dense red-brown gas that 
is very deadly, it is the reward for nitro gone wrong. I used cool water instead of ice because I never 
believed all those warnings. Now I do. I began slowly adding the glycerine - not a change on the 
thermometer. I figured what the hell, I squirted all the glycerine in, stirred it up, checked for a 
temperature rise, and removed it from the coolant water. I set it on the dresser and stepped out for a 
minute. When next I looked down the hall and into my back bedroom, a plume of red smoke and acid 
was shooting out of the flask with increasing intensity. I knew immediately what trouble I was in. My 
dorm was in a pressurized building so no windows open, that means no ventilation. I rushed in to grab 
my gas mask and back out to evacuate my neighbors, except the faggot next door of course, who shared 
nearby rooms. To make a long story short I earned myself a reputation as a potentially dangerous 
individual and now have small holes in most of my shirts because my laundry was nearby. Read the 
Safety section again. This disastrous decomposition is about the worst thing that can happen during the 



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Megalomania's Method of Making Nitroglycerin 



nitration, only very large industrial quantity batches risk detonation from runaway nitration. 
Nitroglycerin has more names than most, they include its proper name of glycerol trinitrate as well as 
1,2,3-propanetriol trinitrate; glyceryl trinitrate; glycerol nitric acid triester; nitroglycerol; 
trinitroglycerol; glonoin; trinitrin; blasting gelatin; blasting oil; S.N.G.; Adesitrin; Angibid; 
Angiolingual; Anginine; Angorin; Aquo-Trinitrosan; Cardamist; Cordipatch; Coro-Nitro; Corditrine; 
Deponit; Diafusor; Discotrine; Gilucor; GTN; Klavikordal; Lenitral; Lentonitrina; Millisrol; Minitran; 
Myoglycerin; Nitradisc; Nitran; Nitriderm-TTS; Nitro-Bid; Nitrocine; Nitrocontin; Nitroderm TTS; 
Nitrodisc; Nitro-Dur; Nitrofortin; Nitrogard; Nitro-Gesanit; Nitroglin; Nitroglyn; Nitroglyn; Nitrolan; 
Nitrolande; Nitrolar; Nitrolent; Nitrolingual; Nitro Mack; Nitromex; Nitronal; Nitrong; Nitro PRN; 
Nitrorectal; Nitroretard; Nitrosigma; Nitrostat; Nitrozell-retard; Nysconitrine; Percutol; Perlinganit; 
Reminitrol; Suscard; Sustac; Sustonit; Transderm-Nitro; Transiderm-Nitro; Tridil; Trinalgon; 
Trinitrosan; and Vasoglyn. That is quite a list, most are drug names though. 







CHEMICALS 


APPARATUS 




chloroform 


1000-mL beaker 


glycerol 


buret 


nitric acid 


desiccator 


sodium carbonate 


1000-mL Florence flask 




sodium chloride 


graduated cylinder 




sulfuric acid 


separatory funnel 




water 


thermometer 





Prepare a mixture of 200 mL of 98-100% nitric acid and 300 mL of 98-100% sulfuric aci by slowly 
adding one to the other in a 1000-mL beaker . Place the beaker into a salt-ice bath during the mixing so it 
may cool, allow the temperature to drop below 10 °C after mixing. You can keep the cold acid in the salt- 
ice bath or you can transfer the acid mix into a round-bottomed 00-niL Florence 11 as! for better heat 
dispersion. In either case, prepare a fresh salt-ice bath. Because of the possibility of friction, standard 
stirring methods are not advised. Instead, use an aquarium pump to blow air into the acids as a means to 
cool and stir them. Regulate the air flow so the acid is being well stirred yet not spattering out. Using a 
buret suspended above the flask, very slowly add drop by drop 112 mL of lycero that has been 
previously cooled to 15 °C. Carefully monitor the temperature of the reaction at all times, the 
temperature must stay below 20 °C, preferably below 15 °C for extra safety. If at any time the 
temperature goes near this, stop adding glycerin until it cools. You can use the rate of addition to control 
the temperature. If the temperature ever rises above 20 °C it is ruined as no more nitro will be made and 
you are in great danger of the existing nitro detonating. If the temperature goes above 30 °C, there is a 
sudden rise in temperature, or a red gas is noticed, DUMP IT INTO COLD WATER 



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Megalomania's Method of Making Nitroglycerin 



IMMEDIATELY!. Keep a bucket of ice water on hand for this task. After adding all of the glycerin, 
allow the temperature to drop to 15 °C and sit for 15 minutes. Carefully pour the reaction mix into a 
large beaker containing an equal volume of room temperature water . Add this mix to a separatory funnel 
and allow the nitroglycerin to settle out, it will form a layer on the bottom of the funnel. Drain off the 
nitro layer and keep the acid waste layer for further extraction. Place the nitro back into a clean 
separatory funnel and add plenty of 38-45 °C water, mix, then separate. Wash the nitro again, then wash 
with a warm 4% sodium carbonate solution. Wash with warm water three more times. Give it a final 
wash of concentrated sodium chloride solution, and let it sit one day before separating the layers. 
Separate and check the nitro for acidity with litmus paper. If it is still acidic keep washing. It must be 
neutral or it will explode. Dry the neutral nitro over sulfuric acid in a desiccator , this may take several 
days. You will need a aduated cylinder for measuring liquids, and a thermometer to monitor the 
temperature. 

To extract any nitro that may still be in the waste acid, first neutralize the acid with sodium carbonate 
solution. Next add an equal volume of chloroform to the neutral waste acid. Mix well then place it into 
the separatory funnel. Remove the bottom nitro layer and let it stand in the open for one day so the 
chloroform may evaporate. Add this nitro to the washing process above. 

One unit of glycerol will yield about 2.5 of nitro. Exposure to nitroglycerine will cause severe 
headaches. Keep it cool, the warmer it is the more sensitive it is to detonation. Frozen nitro can not be 
detonated therefore it is stable BUT partially frozen nitro is extra sensitive ! Although nitroglycerin is 
very dangerous when confined, it is merely flammable when spread out in the open air. Nitroglycerin 
can be destroyed by boiling in a solution of potassium or sodium hydroxide and ethyl alcohol . 




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Megalomania's Method of Making 2-nitro-2-(m-nitrophenyl)-propanediol-l,3 dinitrate 




2-Nitro-2-(m-Nitrophenyl)-Propanediol-1,3 



Di nitrate 




A 



A 



melting point 
73 °C 


boiling point 
ignites at 270 °C 


2-nitro-2-(m-nitrophenyl)- 
propanediol-1,3 dinitrate 


molecular mass 
332.19 g/mol 


density 
? g/mL 


table key 


sensitivity 

low 


chemical formula 
(0 2 N)C 6 H 4 C(N0 2 )(CH 2 0N0 2 ) 


explosive velocity 
? m/s 


estimated cost 

$?.00/g 




Another chemical name for this compound is 2-nitro-2-(3'-nitrophenyl)-propane-l,3-diol dinitrate. 
This compound is rather stable, it will not explode when heated, only ignite. It has about 1 14% the 
explosive strength of TNT while being more stable. This substance takes the form of colorless crystals. 
This procedure is brought to you by those wacky scientists Fieser and Gates from the days of yore in 
1946. 









CHEMICALS 


APPARATUS 


ethvl alcohol 


50-mL beaker 


nitric acid 


sereological pipet 


2-nitro-2-(m-nitrophenvl)-propanediol- 1 ,3 





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Megalomania's Method of Making 2-nitro-2-(m-nitrophenyl)-propanediol-l,3 dinitrate 



sulfuric acid 
urea 
water 



Prepare a mixture of 0.4 mL of 95% sulfuric acid and 0. 15 mL of 70% nitric acid in a 50-mL beaker , 
cool this mixture in a salt-ice bath. Before mixing the acids, add a small amount of urea to the nitric acid 
to remove any nitrous acid contamination. Slowly add 200 mg of 2-nitro-2-(m-nitrophenyl)-propanediol- 
1,3 , then allow the reaction to commence for 10 minutes. After this time, drown the contents of the 
beaker with ice water. A heavy oil should separate, collect this oil and add a few mL of ethyl alcohol . 
Crystals of 2-nitro-2-(m-nitrophenyl)-propanediol-l,3 dinitrate form over a period of 2 weeks, 
whereupon they can be filtered to collect the crystals and dried. A second recrystallization from alcohol 
will yield a very pure product. You will need a sereological pipet for measuring liquids. 




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Megalomania's Controversial Chem Lab ©1997-2004 /2-nitro-2-(m-nitrophenyl)-propanediol-l,3 
dinitrate/ revised January 31, 2004 



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